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_7112440
_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 Cl P, C H2 Cl2, 0.69 (Br), 0.31 (Cl)'
_chemical_formula_sum            'C19 H17 Br0.69 Cl3.32 P'
_chemical_formula_weight         448.71
_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                   15.9738(2)
_cell_length_b                   15.9738(2)
_cell_length_c                   15.9738(2)
_cell_measurement_reflns_used    5113
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.3045
_cell_measurement_theta_min      2.8456
_cell_volume                     4075.91(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 0.991
_diffrn_measured_fraction_theta_max 0.942
_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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12333
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         29.37
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    1.917
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90662
_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            colourless
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1811.0
_exptl_crystal_size_max          0.2921
_exptl_crystal_size_mid          0.2261
_exptl_crystal_size_min          0.2163
_refine_diff_density_max         1.161
_refine_diff_density_min         -1.846
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1773
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0604P)^2^+7.7690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1251
_reflns_number_gt                1495
_reflns_number_total             1773
_reflns_threshold_expression     I>2\s(I)
_cod_duplicate_entry             7108843
_cod_data_source_file            c2cc38363b.txt
_cod_data_source_block           nik39
_cod_database_code               7112440