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_4319274
_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_structural
;

 [{MeC(2-C5H4N)(CH2NSiMe3)2}Ti(NBu-t)(py)]

;
_chemical_formula_sum            'C24 H43 N5 Si2 Ti'
_chemical_formula_weight         505.71
_chemical_name_common
;

 [{(2-C5H4N)CMe(CH2NSiMe3)2}Ti(Nt-Bu)(py)]

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'initially placed geometrically'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.63(3)
_cell_angle_beta                 106.61(3)
_cell_angle_gamma                105.40(2)
_cell_formula_units_Z            2
_cell_length_a                   9.535(3)
_cell_length_b                   10.125(3)
_cell_length_c                   15.948(3)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      35.5
_cell_measurement_theta_min      27.9
_cell_volume                     1416.1(7)
_computing_cell_refinement       'STADI-4 version 1.06a (Stoe & Cie, 1996a)'
_computing_data_collection       'STADI-4 version 1.06a (Stoe & Cie, 1996a)'
_computing_data_reduction        'X-RED version 1.08 (Stoe & Cie, 1996b)'
_computing_molecular_graphics    'SHELXTL/PC version 5.03 (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_measurement_device       'Stoe Stadi-4 four-circle'
_diffrn_measurement_method       omega/theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0267
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7218
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        'variation +/-5'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.407
_exptl_absorpt_correction_T_max  0.886
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_type   'numerical integration'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'trigonal prism'
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.30
_refine_diff_density_rms         0.06
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.025
_refine_ls_goodness_of_fit_obs   1.033
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_restrained_S_obs      1.033
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_obs          0.0416
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.049)^2^+1.615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1084
_refine_ls_wR_factor_obs         0.1011
_reflns_number_observed          4308
_reflns_number_total             4983
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0005644_2.cif
_cod_data_source_block           COMPOUND_3a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_angle_publ_flag' value 'Yes' changed to 'yes' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (10 times).

'_geom_bond_publ_flag' value 'Yes'
changed to 'yes' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (6
times).

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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.049)^2^+1.615P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.049)^2^+1.615P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319274