Characterisation of the tetrahalophosphonium cations PBrnI4 − n+ (0 ≤ n ≤ 4) by 31P MAS NMR, IR and Raman spectroscopy and the crystal structures of PI4+AlCl4−, PI4+AlBr4− and PI4+GaI4−
Christoph Aubauer; Martin Kaupp; Thomas M. Klapötke; Heinrich Nöth; Holger Piotrowski; Wolfgang Schnick; Jürgen Senker; Max Suter; J. Chem. Soc., Dalton Trans.  (2001) 1880–1889; doi:10.1039/b101197i

data_7010619
_publ_section_title
;
 Characterisation of the tetrahalophosphonium cations
 PBrnI4&#x00A0;&#x2212;&#x00A0;n+
 (0&#x00A0;&#x2264;&#x00A0;n&#x00A0;&#x2264;&#x00A0;4) by 31P MAS NMR,
 IR and Raman spectroscopy and the crystal structures of
 PI4+AlCl4&#x2212;, PI4+AlBr4&#x2212; and PI4+GaI4&#x2212;
;
_journal_issue                   12
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1880
_journal_page_last               1889
_journal_paper_doi               10.1039/b101197i
_journal_year                    2001
_chemical_formula_sum            'Al Br4 I4 P'
_chemical_formula_weight         885.19
_chemical_name_systematic        tetraiodophosphonium-tetrabromoaluminate
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-CIF-file updated by CIFRTF'
_cell_angle_alpha                90
_cell_angle_beta                 91.832(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.6475(8)
_cell_length_b                   16.471(2)
_cell_length_c                   14.5339(19)
_cell_measurement_temperature    188(2)
_cell_volume                     1590.5(3)
_computing_cell_refinement       'SMART (V4.C50)'
_computing_data_collection       'SMART (V4.C50)'
_computing_data_reduction        'SAINT (V4.D50)'
_computing_molecular_graphics    'XP (SHELXTL-Ver.5)'
_computing_publication_material  'SHELXL (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      188(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Siemens SMART Area-detector'
_diffrn_measurement_method       Hemisphere
_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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6541
_diffrn_reflns_theta_full        22.71
_diffrn_reflns_theta_max         22.71
_diffrn_reflns_theta_min         1.87
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    17.996
_exptl_absorpt_correction_T_max  0.0666
_exptl_absorpt_correction_T_min  0.0298
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needls
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.873
_refine_diff_density_min         -1.840
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         2056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+14.9708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1145
_reflns_number_gt                1673
_reflns_number_total             2056
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b101197i.txt
_cod_data_source_block           d:\r?ntgen\auba5\auba5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_refine_ls_hydrogen_treatment' value 'mixed ' changed to
'mixed' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'geometrically' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7010619