#------------------------------------------------------------------------------
#$Date: 2019-11-23 20:01:27 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234756 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/21/7702108.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7702108
loop_
_publ_author_name
'Hausmann, David'
'Köppe, Ralf'
'Wolf, Silke'
'Roesky, Peter W.'
'Feldmann, Claus'
_publ_section_title
;
 Ionic-liquid-assisted synthesis of the phosphorus interhalides
 [PBr₄][IBr₂] and
 [PBr₄][I₅Br₇].
;
_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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0837P)²+0.0000P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
I1 I 0.32606(7) 0.2500 0.61456(4) 0.0441(2) Uani 1 2 d S
Br1 Br 0.09316(12) 0.2500 0.70633(8) 0.0562(3) Uani 1 2 d S
Br2 Br 0.58312(11) 0.2500 0.50895(6) 0.0459(3) Uani 1 2 d S
Br3 Br -0.22634(9) -0.02486(10) 0.61435(5) 0.0524(3) Uani 1 1 d .
Br4 Br 0.09436(12) -0.2500 0.58341(8) 0.0578(3) Uani 1 2 d S
Br5 Br -0.06775(12) -0.2500 0.79284(7) 0.0533(3) Uani 1 2 d S
P1 P -0.1047(3) -0.2500 0.65268(15) 0.0428(5) Uani 1 2 d S
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.0473(4) 0.0441(3) 0.0410(3) 0.000 -0.0020(2) 0.000
Br1 0.0495(6) 0.0632(6) 0.0559(6) 0.000 0.0052(4) 0.000
Br2 0.0474(5) 0.0458(5) 0.0444(5) 0.000 0.0024(3) 0.000
Br3 0.0551(5) 0.0451(4) 0.0570(4) 0.0003(3) -0.0002(3) 0.0002(3)
Br4 0.0514(6) 0.0662(7) 0.0558(6) 0.000 0.0087(4) 0.000
Br5 0.0564(6) 0.0606(6) 0.0429(5) 0.000 -0.0028(4) 0.000
P1 0.0463(12) 0.0419(11) 0.0401(11) 0.000 -0.0008(9) 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C6DT03303B 2016
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Br1 I1 Br2 178.91(4) . .
Br3 P1 Br3 106.30(12) . 7
Br3 P1 Br5 110.72(8) . .
Br3 P1 Br5 110.72(8) 7 .
Br3 P1 Br4 109.62(8) . .
Br3 P1 Br4 109.62(8) 7 .
Br5 P1 Br4 109.81(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Br1 2.5823(13) .
I1 Br2 2.8853(12) .
Br3 P1 2.1298(18) .
Br4 P1 2.137(3) .
Br5 P1 2.135(3) .
P1 Br3 2.1298(18) 7
