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_1543709
_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         '2(C54 H72 Br N4 P2), Br6 Sn, C4 H8 O'
_chemical_formula_sum            'C112 H152 Br8 N8 O P4 Sn'
_chemical_formula_weight         2508.26
_chemical_name_systematic
;
 [P2(IPr)2Br]2[SnBr6]*THF
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 1'
_symmetry_space_group_name_Hall  'I -2ya'
_symmetry_space_group_name_H-M   'I 1 a 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                 111.3750(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5603(2)
_cell_length_b                   26.1169(2)
_cell_length_c                   22.7679(2)
_cell_measurement_reflns_used    49187
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.0560
_cell_measurement_theta_min      3.3690
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_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)
;
_computing_molecular_graphics    'WinGX (Farrugia, 2005)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0228
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            72532
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.148
_diffrn_reflns_theta_min         3.384
_exptl_absorpt_coefficient_mu    5.708
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88147
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             5112
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.294
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.459(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1240
_refine_ls_number_reflns         18569
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+17.8202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                18313
_reflns_number_total             18569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc02343f2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        11938.48(19)
_cod_database_code               1543709
_shelx_estimated_absorpt_t_min   0.599
_shelx_estimated_absorpt_t_max   0.599
_shelxl_version_number           2013-4
_shelx_res_checksum              14573
_solvent_exptl_crystal_recrystallization_method THF