2-Pyridonate Titanium Complexes for Chemoselectivity. Accessing Intramolecular Hydroaminoalkylation over Hydroamination
Chong, Eugene; Schafer, Laurel L.; Organic Letters 15 (2013) 6002–; doi:10.1021/ol402890m

data_1513135
_publ_section_title
;
 2-Pyridonate Titanium Complexes for Chemoselectivity. Accessing
 Intramolecular Hydroaminoalkylation over Hydroamination
;
_journal_issue                   23
_journal_name_full               'Organic Letters'
_journal_page_first              6002
_journal_paper_doi               10.1021/ol402890m
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C26 H28 N4 O2 Ti, C6 H6'
_chemical_formula_sum            'C32 H34 N4 O2 Ti'
_chemical_formula_weight         554.51
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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                 97.520(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.2081(5)
_cell_length_b                   13.8771(4)
_cell_length_c                   25.5319(8)
_cell_measurement_reflns_used    8138
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.488
_cell_measurement_theta_min      2.412
_cell_volume                     5693.3(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            39243
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.61
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.336
_exptl_absorpt_correction_T_max  0.9350
_exptl_absorpt_correction_T_min  0.8921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2336
_exptl_crystal_recrystallization_method benzene/pentane
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         6543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+5.6123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0879
_reflns_number_gt                4947
_reflns_number_total             6543
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ol402890m_si_002.cif
_cod_data_source_block           ls254_0m
_cod_original_cell_volume        5693.3(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1513135