Alkylation, Cation Formation, and Insertion Reactions in Titanium Tris(ketimide) Complexes
Ferreira, M. João; Matos, Inês; Ascenso, José R.; Duarte, M. Teresa; Marques, M. Mercês; Wilson, Claire; Martins, Ana M.; Organometallics 26 (2007) 119–; doi:10.1021/om060554w

data_4072465
_publ_section_title
;
 Alkylation, Cation Formation, and Insertion Reactions in Titanium
 Tris(ketimide) Complexes
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              119
_journal_paper_doi               10.1021/om060554w
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C54 H90 F11 N6 P Ti3'
_chemical_formula_sum            'C54 H90 F11 N6 P Ti3'
_chemical_formula_weight         1206.99
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                90.000(5)
_cell_angle_beta                 92.643(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   12.486(5)
_cell_length_b                   13.689(5)
_cell_length_c                   39.421(5)
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.45
_cell_measurement_theta_min      2.47
_cell_volume                     6731(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.2165
_diffrn_reflns_av_sigmaI/netI    0.1680
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            68686
_diffrn_reflns_theta_full        23.45
_diffrn_reflns_theta_max         23.45
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.0332(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         9451
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1905
_refine_ls_R_factor_gt           0.0945
_refine_ls_shift/su_max          0.109
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1342P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2153
_refine_ls_wR_factor_ref         0.2476
_reflns_number_gt                4898
_reflns_number_total             9451
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060554wsi20060626_062801.cif
_cod_data_source_block           compound3
_cod_database_code               4072465