Group 4 Imido Complexes Stabilized by a Tridentate Diamido-Donor Ligand
Alexander J. Blake; Philip E. Collier; Lutz H. Gade; Philip Mountford; Julian Lloyd; Stephen M. Pugh; Martin Schubart; Michael E. G. Skinner; Dominique J. M. Trösch; Inorganic Chemistry 40 (2001) 870–877; doi:10.1021/ic0005644

data_4319276
_publ_contact_author
;
 Professor L H Gade
 Laboratoire de Chimie Organometallique et de Catalyse
 Institut Le Bel
 Universite Louis Pasteur
 4 rue Blaise Pascal
 67070 Strasbourg Cedex
 FRANCE
;
_publ_contact_author_email       Gade@chimie.u-strasbg.fr
_publ_section_title
;
 Group 4 Imido Complexes Stabilized by a Tridentate Diamido-Donor Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              870
_journal_page_last               877
_journal_paper_doi               10.1021/ic0005644
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         ' C19 H38 N4 Si2 Ti1 '
_chemical_formula_sum            'C19 H38 N4 Si2 Ti'
_chemical_formula_weight         426.61
_chemical_name_systematic
;

 [{(2-NC5H4)CMe(CH2NSiMe3)2}Ti(N-t-Bu)]

;
_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 methods (SIR92)'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.39(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4.0
_cell_length_a                   11.934(9)
_cell_length_b                   14.011(11)
_cell_length_c                   15.255(11)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    220(1)
_cell_measurement_theta_max      11.0
_cell_measurement_theta_min      10.0
_cell_volume                     2551(3)
_computing_cell_refinement       'STADI4 (Stoe & Cie, 1997a)'
_computing_data_collection       'STADI4 (Stoe & Cie, 1997a)'
_computing_data_reduction
;

 X-RED (Stoe & Cie, 1997b)

 CRYSTALS (Watkin et al, 1996)

;
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1994)'
_computing_publication_material
;

CRYSTALS Issue 10 (Watkin et al, 1996)

;
_computing_structure_refinement
;

CRYSTALS Issue 10 (Watkin et al, 1996)

;
_computing_structure_solution    'SIR92 (Altomare, et al, 1994)'
_diffrn_ambient_temperature      220(1)
_diffrn_measurement_device       'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
; 

 Scan width (omega) = 2.88 - 2.97, theta:omega scans

;
_diffrn_radiation_collimation    '0.5 mm'
_diffrn_radiation_detector       'NaI(Tl) scintillation counter'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  90
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.11
_diffrn_reflns_av_sigmaI/netI    0.2407
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4412
_diffrn_reflns_theta_max         22.51
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        '14.4 (linear decay)'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.44
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.925
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.75
_refine_diff_density_min         -0.96
_refine_ls_abs_structure_Flack   'not required'
_refine_ls_extinction_coef       'not required'
_refine_ls_extinction_method     'none required'
_refine_ls_goodness_of_fit_obs   1.1517
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         1660
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.1067
_refine_ls_shift/esd_max         0.004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      'Chebychev polynomial'
_refine_ls_wR_factor_obs         0.0847
_reflns_d_resolution_high        0.928
_reflns_d_resolution_low         7.831
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_observed          1660
_reflns_number_total             3336
_reflns_observed_criterion       >2.00\s(I)
_cod_data_source_file            ic0005644_4.cif
_cod_data_source_block           COMPOUND_6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        2550.8(22)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C19 H38 N4 Si2 Ti1 '
_cod_database_code               4319276