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_4074907
_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         '2(C45 H85 Cl3 Hf N2 O Si6), 0.5(C6 H14)'
_chemical_formula_sum            'C93 H177 Cl6 Hf2 N4 O2 Si12'
_chemical_formula_weight         2290.16
_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                74.6796(8)
_cell_angle_beta                 82.5888(4)
_cell_angle_gamma                77.1249(5)
_cell_formula_units_Z            2
_cell_length_a                   11.65970(10)
_cell_length_b                   18.3005(2)
_cell_length_c                   28.9162(3)
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.18
_cell_volume                     5785.06(10)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            48984
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    2.099
_exptl_absorpt_correction_T_max  0.5716
_exptl_absorpt_correction_T_min  0.5716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2386
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1119
_refine_ls_number_reflns         20242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+6.3078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0464
_refine_ls_wR_factor_ref         0.0477
_reflns_number_gt                18394
_reflns_number_total             20242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0509948si20060125_122149.cif
_cod_data_source_block           HfCl3nacnacthf_3c
_cod_database_code               4074907