Pyridonate-Supported Titanium(III). Benzylamine as an Easy-To-Use Reductant
Chong, Eugene; Xue, Wei; Storr, Tim; Kennepohl, Pierre; Schafer, Laurel L.; Organometallics 34 (2015) 4941–; doi:10.1021/acs.organomet.5b00469

data_4087663
_publ_section_title
;
 Pyridonate-Supported Titanium(III). Benzylamine as an Easy-To-Use
 Reductant
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4941
_journal_paper_doi               10.1021/acs.organomet.5b00469
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C47 H42 N5 O3 Ti'
_chemical_formula_sum            'C47 H42 N5 O3 Ti'
_chemical_formula_weight         772.75
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 113.209(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7413(8)
_cell_length_b                   24.558(2)
_cell_length_c                   14.764(1)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25.4035
_cell_measurement_theta_min      2.5125
_cell_volume                     3912.6(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            45253
_diffrn_reflns_theta_full        25.46
_diffrn_reflns_theta_max         25.46
_diffrn_reflns_theta_min         1.66
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  0.9763
_exptl_absorpt_correction_T_min  0.9459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            dark-orange
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1620
_exptl_crystal_recrystallization_method
'slow diffusion of pentane into toluene, room temperature'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         7125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0325P)^2^+3.5929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0961
_reflns_number_gt                5369
_reflns_number_total             7125
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om5b00469_si_001.cif
_cod_data_source_block           mo_ls419_0m
_cod_original_cell_volume        3912.6(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4087663