Reduction of Tetravalent Group 4 Metal Complexes Supported by an Extremely Bulky, Unsymmetrically Substituted β-Diketiminato Ligand Leading to the Regioselective CN Bond Cleavage Giving Ring-Contracted Metal-Imido Complexes
Hamaki, Hirofumi; Takeda, Nobuhiro; Tokitoh, Norihiro; Organometallics 25 (2006) 2457–; doi:10.1021/om0509948

data_4074909
_publ_section_title
;
 Reduction of Tetravalent Group 4 Metal Complexes Supported by an
 Extremely Bulky, Unsymmetrically Substituted \b-Diketiminato Ligand
 Leading to the Regioselective CN Bond Cleavage Giving Ring-Contracted
 Metal-Imido Complexes
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2457
_journal_paper_doi               10.1021/om0509948
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C47 H93 Cl2 Li N4 Si6 Zr, C6 H14'
_chemical_formula_sum            'C53 H107 Cl2 Li N4 Si6 Zr'
_chemical_formula_weight         1138.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.7567(19)
_cell_angle_beta                 108.1972(17)
_cell_angle_gamma                102.239(2)
_cell_formula_units_Z            2
_cell_length_a                   12.718(3)
_cell_length_b                   15.788(4)
_cell_length_c                   19.011(5)
_cell_measurement_reflns_used    9081
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.4
_cell_volume                     3427.8(15)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku Mercury'
_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  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28098
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.33
_diffrn_standards_number         36846
_exptl_absorpt_coefficient_mu    0.376
_exptl_absorpt_correction_T_max  0.9286
_exptl_absorpt_correction_T_min  0.8059
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         11929
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0326P)^2^+2.8598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0795
_reflns_number_gt                10983
_reflns_number_total             11929
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0509948si20060125_122149.cif
_cod_data_source_block           LiZrNCl2tmeda_4b
_cod_database_code               4074909