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_4080455
_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         'C44 H49 N5 Ti'
_chemical_formula_sum            'C44 H49 N5 Ti'
_chemical_formula_weight         695.76
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.245(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9392(4)
_cell_length_b                   13.2438(6)
_cell_length_c                   28.9141(12)
_cell_measurement_reflns_used    8177
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4765
_cell_measurement_theta_min      2.5715
_cell_volume                     3783.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            37188
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.264
_exptl_absorpt_correction_T_max  0.9386
_exptl_absorpt_correction_T_min  0.8808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         8654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0397P)^2^+1.9598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                6779
_reflns_number_total             8654
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om3012695_si_002.cif
_cod_data_source_block           ls341_0m
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4080455