Formation of Phosphorus-Nitrogen Bonds by Reduction of a Titanium Phosphine Complex under Molecular Nitrogen
Lara Morello; Peihua Yu; Christopher D. Carmichael; Brian O. Patrick; Michael D. Fryzuk; Journal of the American Chemical Society 127 (2005) 12796–12797; doi:10.1021/ja054467r

data_4111954
_publ_section_title
;
 Formation of Phosphorus-Nitrogen Bonds by Reduction of a Titanium
 Phosphine Complex under Molecular Nitrogen
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12796
_journal_page_last               12797
_journal_paper_doi               10.1021/ja054467r
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C62 H100 N6 P4 Si8 Ti2'
_chemical_formula_weight         1373.88
_chemical_name_systematic
;
 ?
;
_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                 114.884(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.1300(9)
_cell_length_b                   26.7178(10)
_cell_length_c                   27.4226(10)
_cell_measurement_reflns_used    24612
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.55
_cell_measurement_theta_min      2.25
_cell_volume                     16702.7(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 11.76
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Rigaku/ ADSC CCD'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.083
_diffrn_reflns_av_sigmaI/netI    0.1025
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            16401
_diffrn_reflns_theta_full        26.55
_diffrn_reflns_theta_max         26.55
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.418
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_description       needle
_exptl_crystal_F_000             5840
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     708
_refine_ls_number_reflns         16401
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1033P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1795
_refine_ls_wR_factor_ref         0.1979
_reflns_number_gt                9853
_reflns_number_total             16401
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja054467rsi20050706_115858.cif
_cod_data_source_block           mf470
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4111954