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_4087662
_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         'C35 H30 N4 O3 Ti, C4 H8 O'
_chemical_formula_sum            'C39 H38 N4 O4 Ti'
_chemical_formula_weight         674.63
_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                 97.189(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.127(4)
_cell_length_b                   12.565(4)
_cell_length_c                   21.799(8)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.025
_cell_measurement_theta_min      2.4455
_cell_volume                     3295.5(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            68402
_diffrn_reflns_theta_full        30.17
_diffrn_reflns_theta_max         30.17
_diffrn_reflns_theta_min         1.83
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.308
_exptl_absorpt_correction_T_max  0.9006
_exptl_absorpt_correction_T_min  0.8390
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1416
_exptl_crystal_recrystallization_method 'THF, room temperature'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.34
_refine_diff_density_max         1.442
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         9647
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+1.7908P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0972
_reflns_number_gt                8283
_reflns_number_total             9647
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om5b00469_si_001.cif
_cod_data_source_block           ls476_0m
_cod_original_cell_volume        3296(3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4087662