Reactions of Phosphine Oxides with Bromophosphoranimines; Synthesis and Unusual Rearrangements of O-Donor Stabilized Phosphoranimine Cations
Martin Bendle; Keith Huynh; Mairi F. Haddow; Ian Manners; Inorganic Chemistry 50 (2011) 10292–10302; doi:10.1021/ic201360p

data_4326532
_publ_section_title
;
 Reactions of Phosphine Oxides with Bromophosphoranimines; Synthesis and
 Unusual Rearrangements of O-Donor Stabilized Phosphoranimine Cations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10292
_journal_page_last               10302
_journal_paper_doi               10.1021/ic201360p
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C8 H24 N O P2 Si, F6 P'
_chemical_formula_sum            'C8 H24 F6 N O P3 Si'
_chemical_formula_weight         385.28
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 104.734(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.9242(17)
_cell_length_b                   10.7663(14)
_cell_length_c                   24.733(3)
_cell_measurement_reflns_used    6264
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.42
_cell_volume                     3585.9(8)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker ShelXTL'
_computing_publication_material  'Bruker ShelXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            15927
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.448
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.013
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         4111
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+9.6284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1019
_reflns_number_gt                3598
_reflns_number_total             4111
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201360p_si_002_7.cif
_cod_data_source_block           '[4a]PF6'
_cod_original_cell_volume        3585.8(8)
_cod_database_code               4326532