Unexpected Binuclear Bis(phenolato) Titanium (IV) {[(L)Ti(Ph)]2(μ-OEt)2} Assisted by Carbon−Oxygen Bond Cleavage and Alkali-Metal-Containing Titanium(III) Complexes [Ti(L)2·M(solv)2] (M = Li, Na, K; solv = THF, DME)
Zhang, Dao; Organometallics 26 (2007) 4072–; doi:10.1021/om700298f

data_4073384
_publ_section_title
;
 Unexpected Binuclear Bis(phenolato) Titanium (IV) {[(L)Ti(Ph)]2(\m-OEt)2}
 Assisted by Carbon&#x2212;Oxygen Bond Cleavage and
 Alkali-Metal-Containing Titanium(III) Complexes [Ti(L)2&#x00B7;M(solv)2]
 (M = Li, Na, K; solv = THF, DME)
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4072
_journal_paper_doi               10.1021/om700298f
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C54 H80 K O8 Ti'
_chemical_formula_weight         944.18
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 97.077(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.2073(5)
_cell_length_b                   16.3911(5)
_cell_length_c                   20.6690(7)
_cell_measurement_reflns_used    16718
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     5449.0(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(1)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0660
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9514
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.282
_exptl_absorpt_correction_T_max  0.9724
_exptl_absorpt_correction_T_min  0.9670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2036
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.073
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       0.0020(6)
_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   1.169
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         9514
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.1562
_refine_ls_R_factor_gt           0.1468
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+69.1040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3321
_refine_ls_wR_factor_ref         0.3377
_reflns_number_gt                8626
_reflns_number_total             9514
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700298f-file005.cif
_cod_data_source_block           crystals
_cod_database_code               4073384