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_1513137
_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         'C25 H27 N O2 S, C6 H12'
_chemical_formula_sum            'C31 H39 N O2 S'
_chemical_formula_weight         489.71
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.755(2)
_cell_angle_beta                 72.091(2)
_cell_angle_gamma                66.422(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6913(9)
_cell_length_b                   11.550(1)
_cell_length_c                   12.416(1)
_cell_measurement_reflns_used    9807
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.0935
_cell_measurement_theta_min      2.4405
_cell_volume                     1315.33(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX DUO'
_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  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0176
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27285
_diffrn_reflns_theta_full        30.09
_diffrn_reflns_theta_max         30.09
_diffrn_reflns_theta_min         1.75
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_T_max  0.9540
_exptl_absorpt_correction_T_min  0.8801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             528
_exptl_crystal_recrystallization_method 'cyclohexane, cooled to 281 K'
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.31
_refine_diff_density_max         1.168
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         7629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0568P)^2^+0.6019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1077
_reflns_number_gt                6910
_reflns_number_total             7629
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ol402890m_si_002.cif
_cod_data_source_block           mo_ls377_0m
_cod_original_cell_volume        1315.3(3)
_cod_database_code               1513137