Nucleophilic Attack toward Group 4 Metal Complexes Bearing Reactive 1-Aza-1,3-butadienyl and Imido Moieties
Hirofumi Hamaki; Nobuhiro Takeda; Norihiro Tokitoh; Inorganic Chemistry 46 (2007) 1795–1802; doi:10.1021/ic0620844

data_4307603
_publ_contact_author_address
; Institute for Chemical Research
  Kyoto University
  Gokasho, Uji, Kyoto
  611-0011
  Japan
;
_publ_contact_author_email       tokitoh@boc.kuicr.kyoto-u.ac.jp
_publ_contact_author_fax         '81 774 38 3209'
_publ_contact_author_name        'Prof. Dr. Norihiro Tokitoh'
_publ_contact_author_phone       '81 774 38 3200'
_publ_section_title
;
Nucleophilic Attack toward Group 4 Metal Complexes Bearing Reactive
1-Aza-1,3-butadienyl and Imido Moieties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1795
_journal_page_last               1802
_journal_paper_doi               10.1021/ic0620844
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         '2(C46 H82 Cl N3 Si6 Ti), C6 H14'
_chemical_formula_sum            'C98 H178 Cl2 N6 Si12 Ti2'
_chemical_formula_weight         1944.24
_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                106.011(4)
_cell_angle_beta                 90.942(2)
_cell_angle_gamma                108.792(5)
_cell_formula_units_Z            2
_cell_length_a                   12.368(5)
_cell_length_b                   18.983(8)
_cell_length_c                   27.134(10)
_cell_measurement_reflns_used    6840
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.4
_cell_volume                     5758(4)
_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 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0603
_diffrn_reflns_av_sigmaI/netI    0.0998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            45679
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.43
_diffrn_standards_number         62131
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_T_max  0.9656
_exptl_absorpt_correction_T_min  0.8718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2108
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1127
_refine_ls_number_reflns         19830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.0832
_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^)+(0.0893P)^2^+7.5641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1951
_refine_ls_wR_factor_ref         0.2168
_reflns_number_gt                14012
_reflns_number_total             19830
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0620844si20061101_063238_1.cif
_cod_data_source_block           Tipy_7
_cod_database_code               4307603