Synthesis of a phosphine imide bearing a hydrosilane moiety, and its water-driven reduction to a phosphine
Kano, Naokazu; Yanaizumi, Kazuhide; Meng, Xiangtai; Havare, Nizam; Kawashima, Takayuki; Chemical Communications (Cambridge, United Kingdom) 49 (2013) 10373–10375; doi:10.1039/c3cc43955k

data_7109978
_publ_section_title
;
 Synthesis of a phosphine imide bearing a hydrosilane moiety, and its
 water-driven reduction to a phosphine
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   88
_journal_name_full
'Chemical Communications (Cambridge, United Kingdom)'
_journal_page_first              10373
_journal_page_last               10375
_journal_paper_doi               10.1039/c3cc43955k
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C34 H34 N P Si'
_chemical_formula_sum            'C34 H34 N P Si'
_chemical_formula_weight         515.68
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 112.6137(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.002(9)
_cell_length_b                   8.839(5)
_cell_length_c                   20.361(12)
_cell_measurement_reflns_used    4684
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0402
_cell_volume                     2825(3)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 14.5666
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
scan:
Number of images: 600
Slice: -70.0000 - 110.0000
Image width: 0.3000
Exp time: 21.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 45.0000
Phi: 0.0000
XTD: 45.0843
2theta: 19.6674
scan:
Number of images: 600
Slice: -70.0000 - 110.0000
Image width: 0.3000
Exp time: 21.0000
Rotation axis: Omega
Omega: 0.0000
Chi: 45.0000
Phi: 90.0000
XTD: 45.0843
2theta: 19.6674

;
_diffrn_measurement_device
;
Mercury CCD (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC8: Eulerian 3-circle
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0599
_diffrn_orient_matrix_UB_12      0.0094
_diffrn_orient_matrix_UB_13      -0.0196
_diffrn_orient_matrix_UB_21      -0.0234
_diffrn_orient_matrix_UB_22      0.1090
_diffrn_orient_matrix_UB_23      -0.0191
_diffrn_orient_matrix_UB_31      0.0326
_diffrn_orient_matrix_UB_32      0.0140
_diffrn_orient_matrix_UB_33      0.0397
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.1234
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8803
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.04
_diffrn_source_current           40.0000
_diffrn_source_power             2.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  0.9839
_exptl_absorpt_correction_T_min  0.9527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Jacobson R (1988) Private communication
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.790
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         4518
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.790
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+(-0.9400P)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0354
_refine_ls_wR_factor_ref         0.0390
_reflns_number_gt                3520
_reflns_number_total             4518
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc43955k.txt
_cod_data_source_block           sihph2
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7109978