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_1543704
_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         'C27 H36 Br3 N2 P'
_chemical_formula_sum            'C27 H36 Br3 N2 P'
_chemical_formula_weight         659.28
_chemical_name_systematic
;
 (IPr)PBr3
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 108.0790(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.28300(10)
_cell_length_b                   18.30220(10)
_cell_length_c                   15.64950(10)
_cell_measurement_reflns_used    21180
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.1270
_cell_measurement_theta_min      3.8291
_cell_volume                     2799.85(4)
_computing_cell_refinement
;
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_data_collection
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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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_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4102
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_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  0.0198
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31191
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.118
_diffrn_reflns_theta_min         3.829
_exptl_absorpt_coefficient_mu    6.011
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
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Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5822
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+2.6748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0580
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5719
_reflns_number_total             5822
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc02343f2.cif
_cod_data_source_block           shelx
_cod_database_code               1543704
_shelx_estimated_absorpt_t_min   0.304
_shelx_estimated_absorpt_t_max   0.532
_shelxl_version_number           2013-4
_shelx_res_checksum              54723
_solvent_exptl_crystal_recrystallization_method 'THF, hexane'