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_7010617
_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_compound_source
;
crystal provided by C. Aubauer
;
_chemical_formula_moiety         '(Ga I4), (P I4)'
_chemical_formula_sum            'Ga I8 P'
_chemical_formula_weight         1115.932
_chemical_name_common            (PI4)(GaI4)
_chemical_name_systematic        tetraiodophosphonium-tetraiodogallate
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                GaI4_PI4_e187_klapoetke
_audit_creation_date             08-Aug-00
_audit_creation_method           'form98_1/compatible with shelxl97-2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0101(7)
_cell_length_b                   10.4007(7)
_cell_length_c                   15.1835(9)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    200(3)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.4
_cell_volume                     1738.70(19)
_computing_cell_refinement       'Stoe IPDS software (Darmstadt, Germany)'
_computing_data_collection       'Stoe IPDS software (Darmstadt, Germany)'
_computing_data_reduction        'Stoe IPDS software (Darmstadt, Germany)'
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution
;
SIR97 (Cascarano et al.,Acta Crystallogr., Sect A, 1996, C79)
;
_diffrn_ambient_temperature      200(3)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'image-plate area detector'
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'area detection'
_diffrn_radiation_collimation    '0.5 mm collimator'
_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  0.0527
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9490
_diffrn_reflns_theta_full        27.95
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         2.37
_diffrn_source_current           50_mA
_diffrn_source_power             2.75_kW
_diffrn_source_type              'Spellman DF4 Series'
_diffrn_source_voltage           55_kV
_exptl_absorpt_coefficient_mu    15.839
_exptl_absorpt_correction_T_max  0.3692
_exptl_absorpt_correction_T_min  0.0640
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRed, rev. 1.09, Stoe (Darmstadt, Germany)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    4.263(3)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.981
_refine_diff_density_min         -1.753
_refine_diff_density_rms         0.338
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         3879
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0389P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0785
_reflns_number_gt                3142
_reflns_number_total             3879
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b101197i.txt
_cod_data_source_block           e187
_cod_database_code               7010617