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_4080453
_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         'C29 H43 N5 Ti'
_chemical_formula_sum            'C29 H43 N5 Ti'
_chemical_formula_weight         509.55
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 107.040(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.7276(2)
_cell_length_b                   8.5789(2)
_cell_length_c                   16.3989(4)
_cell_measurement_reflns_used    7884
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.964
_cell_measurement_theta_min      2.598
_cell_volume                     1442.95(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16131
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    0.321
_exptl_absorpt_correction_T_max  0.9469
_exptl_absorpt_correction_T_min  0.8757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         7618
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0879
_reflns_number_gt                6384
_reflns_number_total             7618
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om3012695_si_002.cif
_cod_data_source_block           ls313
_cod_original_cell_volume        1442.96(7)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4080453