Direct evidence of a multicentre halogen bond: unexpected contraction of the P-XXX-P fragment in triphenylphosphine dihalides.
Nikitin, Kirill; Müller-Bunz, Helge; Gilheany, Declan; Chemical communications (Cambridge, England) 49 (2013) 1434–1436; doi:10.1039/c2cc38363b

data_7112439
_publ_section_title
;
 Direct evidence of a multicentre halogen bond: unexpected contraction of
 the P-XXX-P fragment in triphenylphosphine dihalides.
;
_journal_issue                   14
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1434
_journal_page_last               1436
_journal_paper_doi               10.1039/c2cc38363b
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C18 H15 Br2 P, C H2 Cl2'
_chemical_formula_sum            'C19 H17 Br2 Cl2 P'
_chemical_formula_weight         507.02
_chemical_name_systematic
;
?
;
_space_group_IT_number           205
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.1626(2)
_cell_length_b                   16.1626(2)
_cell_length_c                   16.1626(2)
_cell_measurement_reflns_used    3784
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.0520
_cell_measurement_theta_min      3.5582
_cell_volume                     4222.15(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3196
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11953
_diffrn_reflns_theta_full        24.10
_diffrn_reflns_theta_max         24.10
_diffrn_reflns_theta_min         3.57
_exptl_absorpt_coefficient_mu    4.168
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.1308
_exptl_crystal_size_mid          0.1037
_exptl_crystal_size_min          0.0976
_platon_squeeze_details
;
PLATON: A.L. Spek, J. Appl. Cryst. 36 (2003), 7-13
PLATON version from 30.03.2011
;
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         1127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0755P)^2^+7.4404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1294
_refine_ls_wR_factor_ref         0.1340
_reflns_number_gt                985
_reflns_number_total             1127
_reflns_threshold_expression     I>2\s(I)
_cod_duplicate_entry             7108842
_cod_data_source_file            c2cc38363b.txt
_cod_data_source_block           nik33sqz
_cod_database_code               7112439