Ionic-liquid-assisted synthesis of the phosphorus interhalides [PBr<sub>4</sub>][IBr<sub>2</sub>] and [PBr<sub>4</sub>][I<sub>5</sub>Br<sub>7</sub>].
Hausmann, David; Köppe, Ralf; Wolf, Silke; Roesky, Peter W.; Feldmann, Claus; Dalton transactions (Cambridge, England : 2003) 45 (2016) 16526–16532; doi:10.1039/c6dt03303b

data_7702108
_publ_section_title
;
 Ionic-liquid-assisted synthesis of the phosphorus interhalides
 [PBr<sub>4</sub>][IBr<sub>2</sub>] and
 [PBr<sub>4</sub>][I<sub>5</sub>Br<sub>7</sub>].
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16526
_journal_page_last               16532
_journal_paper_doi               10.1039/c6dt03303b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         Br4P,Br2I
_chemical_formula_sum            'Br6 I P'
_chemical_formula_weight         637.33
_chemical_name_systematic        '[PBr4][IBr2]'
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   notdet
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc1kntbc
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-01-26 deposited with the CCDC.
2017-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3739(19)
_cell_length_b                   7.5698(15)
_cell_length_c                   15.028(3)
_cell_measurement_reflns_used    9283
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.68
_cell_measurement_theta_min      2.50
_cell_volume                     1066.4(4)
_computing_cell_refinement       'CELL, SELECT (STOE)'
_computing_data_collection       'EXPOSE (STOE)'
_computing_data_reduction        'INTEGRATE (STOE)'
_computing_molecular_graphics    'DIAMOND, Crystal Impact'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'image plate'
_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  0.0894
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9901
_diffrn_reflns_theta_full        29.20
_diffrn_reflns_theta_max         29.20
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    25.560
_exptl_absorpt_correction_T_max  0.1131
_exptl_absorpt_correction_T_min  0.0318
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'(X-RED, Data Reduction Program, Version 1.14, Stoe & Cie GmbH, Darmstadt 1999.; X-SHAPE, Crystal Optimisation for Numerical Absorption Correction, Version 1.06, Stoe & Cie GmbH, Darmstadt 1999.)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.970
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.704
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.306
_refine_ls_extinction_coef       0.0081(9)
_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_ref   1.128
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         1548
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0837P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1373
_reflns_number_gt                1305
_reflns_number_total             1548
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt03303b1.cif
_cod_data_source_block           PBr6I
_cod_original_cell_volume        1066.3(4)
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7702108