Divergent Pathways of C-H Bond Activation: Reactions of (t-Bu3PN)2TiMe2 with Trimethylaluminum
James E. Kickham; Frédéric Guérin; Douglas W. Stephan; Journal of the American Chemical Society 124 (2002) 11486–11494; doi:10.1021/ja0260972

data_4115156
_publ_section_title
;
 Divergent Pathways of C-H Bond Activation: Reactions of (t-Bu3PN)2TiMe2
 with Trimethylaluminum
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11486
_journal_page_last               11494
_journal_paper_doi               10.1021/ja0260972
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C36 H84 Al4 N2 P2 Ti2'
_chemical_formula_weight         810.72
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.82150(10)
_cell_length_b                   18.71910(10)
_cell_length_c                   19.8293(4)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     4759.17(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_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  0.0648
_diffrn_reflns_av_sigmaI/netI    0.0846
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24014
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_T_max  0.152595
_exptl_absorpt_correction_T_min  0.111113
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         8297
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.002
_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          0.1458
_refine_ls_wR_factor_ref         0.1684
_reflns_number_gt                5518
_reflns_number_total             8297
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0260972_s1_1.cif
_cod_data_source_block           '[(??-t-Bu3PN)Ti(?4-C)(AlMe2)(AlMe2(?-Me))]2'
_cod_database_code               4115156