#------------------------------------------------------------------------------
#$Date: 2019-11-23 20:01:27 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234756 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/21/7702109.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_7702109
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         2(Br4P),Br7I5
_chemical_formula_sum            'Br15 I5 P2'
_chemical_formula_weight         1895.09
_chemical_name_systematic        '[PBr4]2[I5Br7]'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   notdet
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc1kntcd
_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                91.12(3)
_cell_angle_beta                 92.47(3)
_cell_angle_gamma                111.88(3)
_cell_formula_units_Z            1
_cell_length_a                   9.2316(18)
_cell_length_b                   9.5736(19)
_cell_length_c                   9.6641(19)
_cell_measurement_reflns_used    6991
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.66
_cell_measurement_theta_min      2.29
_cell_volume                     791.3(3)
_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 0.939
_diffrn_measured_fraction_theta_max 0.935
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3028
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    23.945
_exptl_absorpt_correction_T_max  0.1056
_exptl_absorpt_correction_T_min  0.0078
_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    3.977
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.057
_refine_diff_density_min         -1.766
_refine_diff_density_rms         0.363
_refine_ls_extinction_coef       0.0305(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         3028
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0497
_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/[σ²(Fo²)+(0.0946P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1262
_reflns_number_gt                2439
_reflns_number_total             3028
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt03303b1.cif
_cod_data_source_block           P2Br15I5
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7702109
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.37070(7) 0.77913(8) 0.55497(6) 0.0405(2) Uani 1 1 d .
I2 I 0.66458(7) 0.58173(8) 0.71675(8) 0.0460(2) Uani 1 1 d .
I3 I 1.47848(10) -0.05784(12) 0.87218(11) 0.0553(3) Uani 0.50 1 d P
Br1 Br 0.08996(13) 0.75420(14) 0.61860(11) 0.0479(3) Uani 1 1 d .
Br2 Br 0.67171(12) 0.79322(14) 0.50148(11) 0.0491(3) Uani 1 1 d .
Br3 Br 0.66757(14) 0.39970(17) 0.90658(17) 0.0641(4) Uani 1 1 d .
Br4 Br 1.47848(10) -0.05784(12) 0.87218(11) 0.0553(3) Uani 0.50 1 d P
Br5 Br 0.94730(12) 0.21786(13) 1.03763(10) 0.0437(3) Uani 1 1 d .
Br6 Br 0.90622(13) 0.04575(13) 0.71104(11) 0.0467(3) Uani 1 1 d .
Br7 Br 1.27699(13) 0.23106(17) 0.87699(12) 0.0554(3) Uani 1 1 d .
Br8 Br 1.06356(14) 0.43495(13) 0.74728(11) 0.0485(3) Uani 1 1 d .
P1 P 1.0494(3) 0.2320(3) 0.8420(2) 0.0371(5) Uani 1 1 d .
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 0.0444(4) 0.0456(4) 0.0298(3) 0.0010(2) 0.0029(2) 0.0146(3)
I2 0.0352(3) 0.0495(5) 0.0512(4) -0.0070(3) -0.0021(3) 0.0143(3)
I3 0.0417(4) 0.0571(6) 0.0695(6) 0.0095(4) 0.0066(4) 0.0205(4)
Br1 0.0489(6) 0.0636(8) 0.0368(5) 0.0112(5) 0.0066(4) 0.0266(5)
Br2 0.0425(5) 0.0624(8) 0.0365(5) -0.0048(5) 0.0036(4) 0.0129(5)
Br3 0.0445(6) 0.0605(9) 0.0855(10) 0.0141(7) -0.0078(6) 0.0183(5)
Br4 0.0417(4) 0.0571(6) 0.0695(6) 0.0095(4) 0.0066(4) 0.0205(4)
Br5 0.0434(5) 0.0560(7) 0.0346(5) 0.0051(4) 0.0065(4) 0.0214(5)
Br6 0.0545(6) 0.0463(7) 0.0374(5) -0.0010(4) -0.0034(4) 0.0174(5)
Br7 0.0433(5) 0.0873(9) 0.0441(6) 0.0022(5) 0.0026(4) 0.0344(6)
Br8 0.0608(6) 0.0463(7) 0.0367(5) 0.0062(4) -0.0019(4) 0.0182(5)
P1 0.0392(12) 0.0449(15) 0.0284(11) 0.0016(10) 0.0003(9) 0.0172(11)
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 176.14(4) . .
Br3 I2 Br2 178.22(4) . .
Br4 I3 I3 0.00(7) 2_857 2_857
I1 Br2 I2 92.05(5) . .
Br7 P1 Br8 109.55(13) . .
Br7 P1 Br6 111.47(12) . .
Br8 P1 Br6 108.87(12) . .
Br7 P1 Br5 107.95(12) . .
Br8 P1 Br5 109.99(12) . .
Br6 P1 Br5 109.00(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Br1 2.6141(13) .
I1 Br2 2.8026(14) .
I2 Br3 2.5612(18) .
I2 Br2 2.9169(17) .
I3 Br4 2.640(2) 2_857
I3 I3 2.640(2) 2_857
Br5 P1 2.133(3) .
Br6 P1 2.131(3) .
Br7 P1 2.117(3) .
Br8 P1 2.126(3) .
