Titanium and Niobium Imido Complexes Derived from Diamidoamine Ligands
Philip E. Collier; Stephen M. Pugh; Howard S. C. Clark; Jason B. Love; Alexander J. Blake; F. Geoffrey N. Cloke; Philip Mountford; Inorganic Chemistry 39 (2000) 2001–2005; doi:10.1021/ic991014c

data_4320906
_publ_contact_author
;
 Dr P. Mountford           
 Inorganic Chemistry Laboratory
 South Parks Road
 Oxford
 OX1 3QR
 UK
;
_publ_contact_author_email       Philip.Mountford@chem.ox.ac.uk
_publ_contact_author_fax         '+44 1865 272690'
_publ_contact_author_phone       '+44 1865 272679'
_publ_section_title
;
 Titanium and Niobium Imido Complexes Derived from Diamidoamine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2001
_journal_page_last               2005
_journal_paper_doi               10.1021/ic991014c
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C22 H49 N5 Si3 Ti1 '
_chemical_formula_sum            'C22 H49 N5 Si3 Ti'
_chemical_formula_weight         515.83
_chemical_name_systematic
;
 [Ti(NBu-t){Me3SiN(CH2CH2NSiMe3)2}(py)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 102.26(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.857(4)
_cell_length_b                   19.382(4)
_cell_length_c                   16.339(5)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      12.5
_cell_volume                     3050.3(17)
_computing_cell_refinement       'STADI4 (Stoe & Cie 1995a)'
_computing_data_collection       'STADI4 (Stoe & Cie 1995a)'
_computing_data_reduction
;
 X-RED (Stoe & Cie, 1995b)
 CRYSTALS (Watkin et al, 1996)
;
_computing_molecular_graphics    'CAMERON (Watkin, Prout and Pearce, 1996)'
_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      150(1)
_diffrn_measurement_device       'STOE STADI4 4-circle-diffractometer D092'
_diffrn_measurement_method
; Scan width (omega) = 2.45 - 2.59, scan ratio 2theta:omega = 1.00
  I(Net) and sigma(I) calculated according to Blessing (1987)
;
_diffrn_radiation_collimation    '0.8 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  0.00
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5382
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        9.9
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.41
_exptl_absorpt_correction_T_max  0.8710
_exptl_absorpt_correction_T_min  0.6783
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
    Psi Scan Reflections used    Mu * R = 0.09  

    H   K   L   2Theta   Chi   Imin/Imax
    1  -3  -1     7.7   -73.0    0.737
   -1   4   1     9.5    74.1    0.773
    2  -5  -1    13.4   -80.1    0.834
    1  -7  -1    15.3   -70.2    0.691
    2  -8  -1    18.7   -80.8    0.779
   -2   8   2    19.0    74.1    0.752
    3  -9  -1    22.7   -85.7    0.783
    3 -10  -1    24.5   -85.4    0.830
   -4   9   3    25.5    73.5    0.799
    3 -11  -2    26.4   -79.4    0.770
    4 -13  -2    32.2   -82.6    0.839
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.12
_exptl_crystal_density_meas      ?
_exptl_crystal_description       lozenge
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.580
_exptl_crystal_size_mid          0.437
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.61
_refine_diff_density_min         -0.75
_refine_ls_abs_structure_Flack   'not refined'
_refine_ls_extinction_coef       'not refined'
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_all   0.7200
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4943
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_obs          0.062
_refine_ls_shift/esd_max         0.069901
_refine_ls_structure_factor_coef F**2
_refine_ls_weighting_scheme      'Chebychev polynomial'
_refine_ls_wR_factor_all         0.1231
_refine_ls_wR_factor_obs         0.111
_reflns_d_resolution_high        0.841
_reflns_d_resolution_low         7.972
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_observed          4306
_reflns_number_total             5382
_reflns_observed_criterion       >2.00\s(I)
_cod_data_source_file            ic991014c_2.cif
_cod_data_source_block           COMPOUND_1
_cod_depositor_comments
;
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_primary' value 'direct methods' was changed to
'direct'.

'_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        3050.4(14)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        ' C22 H49 N5 Si3 Ti1 '
_cod_database_code               4320906