Isolation and characterization of the first bis(2-pyridyl)carbyltitanium(IV) complex derived from the C‒O bond cleavage of the alkoxide ligand in Cp*TiMe2(OCMePy2). X-Ray crystal structure of [Cp*Ti(μ-O)(CMePy2)]2 (Cp* = C5Me5)
Rosa Fandos; Carolina Hernández; Antonio Otero; Ana Rodríguez; Maria José Ruiz; Pilar Terreros; J. Chem. Soc., Dalton Trans.  (2002) 11–13; doi:10.1039/b106481a

data_7010992
_publ_section_title
;
 Isolation and characterization of the first
 bis(2-pyridyl)carbyltitanium(IV) complex derived from the C--O bond
 cleavage of the alkoxide ligand in Cp*TiMe2(OCMePy2). X-Ray crystal
 structure of [Cp*Ti(\m-O)(CMePy2)]2 (Cp* = C5Me5)
;
_journal_issue                   1
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              11
_journal_page_last               13
_journal_paper_doi               10.1039/b106481a
_journal_year                    2002
_chemical_formula_sum            'C44 H56 N4 O2 Ti2'
_chemical_formula_weight         764.70
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_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                 103.960(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.034(2)
_cell_length_b                   10.346(3)
_cell_length_c                   16.992(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     1882.5(10)
_computing_cell_refinement       'Nonius (control program)'
_computing_data_collection       'Nonius (control program)'
_computing_data_reduction        'XRAY80 (Stewart, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'four circle diffractometer Nonius-Mach3'
_diffrn_measurement_method       '\w/2\q scans'
_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    0.1562
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2288
_diffrn_reflns_theta_full        22.00
_diffrn_reflns_theta_max         22.00
_diffrn_reflns_theta_min         2.32
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.468
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.0015(12)
_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   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         2288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1913
_refine_ls_R_factor_gt           0.0971
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1135P)^2^+4.8819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2134
_refine_ls_wR_factor_ref         0.2910
_reflns_number_gt                1051
_reflns_number_total             2288
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b106481a.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7010992