Insertion Reactions into the Metal–Alkyl and Metal–Amido Bonds of 1,3-Di(silyl-η-amido)cyclopentadienyl Titanium and Zirconium Complexes
Cano, Jesús; Sudupe, María; Royo, Pascual; Mosquera, Marta E. G.; Organometallics 24 (2005) 2424–2432; doi:10.1021/om048984e

data_1100800
_publ_section_title
;
 Insertion Reactions into the Metal--Alkyl and Metal--Amido Bonds of
 1,3-Di(silyl-\h-amido)cyclopentadienyl Titanium and Zirconium Complexes
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2424
_journal_page_last               2432
_journal_paper_doi               10.1021/om048984e
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C36 H54 N4 Si2 Ti1'
_chemical_formula_sum            'C36 H54 N4 Si2 Ti'
_chemical_formula_weight         646.91
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_cell_angle_alpha                98.372(6)
_cell_angle_beta                 102.866(10)
_cell_angle_gamma                99.863(7)
_cell_formula_units_Z            2
_cell_length_a                   9.7722(10)
_cell_length_b                   11.3369(4)
_cell_length_c                   17.0066(16)
_cell_measurement_reflns_used    120
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      21.149
_cell_measurement_theta_min      5.123
_cell_volume                     1776.2(3)
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_sigmaI/netI    0.0986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15135
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.338
_exptl_absorpt_correction_T_max  1.242
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.412
_exptl_crystal_size_mid          0.396
_exptl_crystal_size_min          0.194
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         8058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0614
_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^)+(0.0706P)^2^+1.4230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1466
_refine_ls_wR_factor_ref         0.1654
_reflns_number_gt                5192
_reflns_number_total             8058
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               1100800