2-Aminopyridinate Titanium Complexes for the Catalytic Hydroamination of Primary Aminoalkenes
Chong, Eugene; Qayyum, Sadaf; Schafer, Laurel L.; Kempe, Rhett; Organometallics 32 (2013) 1858–; doi:10.1021/om3012695

data_4080452
_publ_section_title
;
 2-Aminopyridinate Titanium Complexes for the Catalytic Hydroamination of
 Primary Aminoalkenes
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1858
_journal_paper_doi               10.1021/om3012695
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C38 H61 N5 Ti'
_chemical_formula_sum            'C38 H61 N5 Ti'
_chemical_formula_weight         635.79
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.448(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.9251(8)
_cell_length_b                   21.6550(11)
_cell_length_c                   9.3611(5)
_cell_measurement_reflns_used    8177
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.487
_cell_measurement_theta_min      2.196
_cell_volume                     3760.1(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            29679
_diffrn_reflns_theta_full        26.77
_diffrn_reflns_theta_max         26.77
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.259
_exptl_absorpt_correction_T_max  0.9569
_exptl_absorpt_correction_T_min  0.8897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         7979
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.060
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+3.7998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1291
_reflns_number_gt                6140
_reflns_number_total             7979
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om3012695_si_002.cif
_cod_data_source_block           ls288
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4080452