Synthesis, structure, and reactivity of tris(amidate) mono(amido) and tetrakis(amidate) complexes of group 4 transition metals.
Payne, Philippa R.; Thomson, Robert K.; Medeiros, Diane M.; Wan, Geoff; Schafer, Laurel L.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 15670–15677; doi:10.1039/c3dt51868j

data_7023736
_publ_section_title
;
 Synthesis, structure, and reactivity of tris(amidate) mono(amido) and
 tetrakis(amidate) complexes of group 4 transition metals.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15670
_journal_page_last               15677
_journal_paper_doi               10.1039/c3dt51868j
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C47 H48 N4 O3 Ti'
_chemical_formula_sum            'C47 H48 N4 O3 Ti'
_chemical_formula_weight         764.79
_chemical_name_common
'tris(N-(2,6-dimethylphenyl)benzamidate) mono(dimethylamido) titanium, 1'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_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                 90.418(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.942(3)
_cell_length_b                   10.581(1)
_cell_length_c                   31.085(3)
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.705
_cell_measurement_theta_min      2.190
_cell_volume                     8203.5(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            40442
_diffrn_reflns_theta_full        28.76
_diffrn_reflns_theta_max         28.76
_diffrn_reflns_theta_min         1.31
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.254
_exptl_absorpt_correction_T_max  0.9656
_exptl_absorpt_correction_T_min  0.8662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3232
_exptl_crystal_recrystallization_method 'Layered pentanes/toluene'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         10639
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0384P)^2^+16.0980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1164
_reflns_number_gt                8441
_reflns_number_total             10639
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3dt51868j.txt
_cod_data_source_block           ls458a
_cod_original_cell_volume        8203.0(24)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7023736