New Silylated Iminophosphorano(amino)phosphines Me3SiNPPh2N(R)PPh2 (R = Et, nPr, nBu). Crystal and Molecular Structure of Trimethylsilyliminophosphorano(propylamino)diphenylphosphine Me3SiNPPh2N(nPr)PPh2. Further Oxidative Derivatization with S, Se, and Azides, Titanium(IV) Transmetalation of the Imine, and Syntheses of Rhodium(I), Palladium(II), and Platinum(II) Complexes of These Iminophosphorano(amino)phosphines
Maravanji S. Balakrishna; S. Teipel; A. Alan Pinkerton; Ronald G. Cavell; Inorganic Chemistry 40 (2001) 1802–1808; doi:10.1021/ic000878r

data_4319494
_publ_contact_author_address
; Department of Chemistry
  University of Alberta
  Edmonton Alberta T6G 2G2
  Canada
;
_publ_contact_author_email       Ron.Cavell@ualberta.ca
_publ_contact_author_fax         '+1 780 492 8231'
_publ_contact_author_name        'Dr Ronald G Cavell'
_publ_contact_author_phone       '+1 780 492 5310'
_publ_section_title
;
 New Silylated Iminophosphorano(amino)phosphines Me3SiNPPh2N(R)PPh2 (R =
 Et, nPr, nBu). Crystal and Molecular Structure of
 Trimethylsilyliminophosphorano(propylamino)diphenylphosphine
 Me3SiNPPh2N(nPr)PPh2. Further Oxidative Derivatization with S, Se, and
 Azides, Titanium(IV) Transmetalation of the Imine, and Syntheses of
 Rhodium(I), Palladium(II), and Platinum(II) Complexes of These
 Iminophosphorano(amino)phosphines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1802
_journal_page_last               1808
_journal_paper_doi               10.1021/ic000878r
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C30 H36 N2 P2 Si'
_chemical_formula_weight         514.67
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL template'
_cell_angle_alpha                90.00
_cell_angle_beta                 101.05(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.235(1)
_cell_length_b                   16.802(2)
_cell_length_c                   17.075(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    221(1)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      9.0
_cell_volume                     2881.9(6)
_computing_cell_refinement       'CAD4 (Enraf-Nonius, 1977)'
_computing_data_collection       'CAD4 (Enraf-Nonius, 1977)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'MolEN (Fair, 1990)'
_computing_structure_refinement  'MolEN (Fair, 1990)'
_computing_structure_solution
'MULTAN (Main, Fiske, Hull Lessinger, Germain, DeClerq, Woolfson, 1980)'
_diffrn_ambient_temperature      221(1)
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       '\q-2\q scans'
_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  0.036
_diffrn_reflns_av_sigmaI/netI    0.0726
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6193
_diffrn_reflns_theta_max         26.0
_diffrn_reflns_theta_min         2.0
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.19
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.31(4)
_refine_diff_density_min         -0.10(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.42
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         3531
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.044
_refine_ls_shift/su_max          0.010
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'calc w=4Fo^2/\s^2^(Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.054
_reflns_number_gt                3531
_reflns_number_total             5853
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            ic000878r.cif
_cod_data_source_block           C30H36N2P2Si
_cod_original_cell_volume        2882.9(5)
_cod_database_code               4319494
_exptl_absorpt_coefficient_mm    0.21