Synthesis and Reactivity of Phosphine-Stabilized Phosphoranimine Cations, [R3P.PR'2=NSiMe3]+
Keith Huynh; Alan J. Lough; Michelle A. M. Forgeron; Martin Bendle; Alejandro Presa Soto; Roderick E. Wasylishen; Ian Manners; Journal of the American Chemical Society 131 (2009) 7905–7916; doi:10.1021/ja900256g

data_4104481
_publ_section_title
;
 Synthesis and Reactivity of Phosphine-Stabilized Phosphoranimine Cations,
 [R3P.PR'2=NSiMe3]+
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7905
_journal_page_last               7916
_journal_paper_doi               10.1021/ja900256g
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C11 H30 Br N P2 Si'
_chemical_formula_weight         346.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                118.170(2)
_cell_angle_beta                 104.297(3)
_cell_angle_gamma                90.164(2)
_cell_formula_units_Z            8
_cell_length_a                   14.0798(7)
_cell_length_b                   17.0889(8)
_cell_length_c                   18.0705(6)
_cell_measurement_temperature    293(2)
_cell_volume                     3677.7(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0772
_diffrn_reflns_av_sigmaI/netI    0.0907
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42338
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    2.457
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1456
_refine_diff_density_max         1.231
_refine_diff_density_min         -1.477
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.564
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         16600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.564
_refine_ls_R_factor_all          0.1966
_refine_ls_R_factor_gt           0.1478
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4397
_refine_ls_wR_factor_ref         0.4493
_reflns_number_gt                10672
_reflns_number_total             16600
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja900256g_si_003.cif
_cod_data_source_block           k06168
_cod_database_code               4104481