N-heterocyclic carbene induced reductive coupling of phosphorus tribromide. Isolation of a bromine bridged P‒P bond and its subsequent reactivity.
Waters, Jordan; Everitt, Thomas; Myers, William; Goicoechea, Jose M.; Chem. Sci.  (2016) –; doi:10.1039/C6SC02343F

data_1543705
_publ_section_title
;
 N-heterocyclic carbene induced reductive coupling of phosphorus
 tribromide. Isolation of a bromine bridged P--P bond and its subsequent
 reactivity.
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C6SC02343F
_journal_year                    2016
_chemical_formula_moiety         'C54 H72 Br3 N4 P2, Br, 3(C4 H8 O)'
_chemical_formula_sum            'C66 H96 Br4 N4 O3 P2'
_chemical_formula_weight         1375.04
_chemical_name_systematic
;
 [{(IPr)PBr}2Br]Br*3THF
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-05-19 deposited with the CCDC.
2016-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                76.130(3)
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_cell_length_b                   15.5789(7)
_cell_length_c                   18.8569(6)
_cell_measurement_reflns_used    19750
_cell_measurement_temperature    150(2)
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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_computing_molecular_graphics    'WinGX (Farrugia, 2005)'
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_diffrn_ambient_temperature      150(2)
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_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_k_min       -19
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_diffrn_reflns_theta_full        67.679
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_exptl_absorpt_coefficient_mu    3.708
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_exptl_absorpt_correction_type   multi-scan
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CrysAlisPro, Agilent Technologies,
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Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             1428
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
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_refine_diff_density_min         -1.726
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_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0469
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0758P)^2^+8.1166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1358
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13094
_reflns_number_total             13975
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc02343f2.cif
_cod_data_source_block           shelx
_cod_database_code               1543705
_shelx_estimated_absorpt_t_min   0.403
_shelx_estimated_absorpt_t_max   0.524
_shelxl_version_number           2013-4
_shelx_res_checksum              7541
_solvent_exptl_crystal_recrystallization_method THF