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_4320905
_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_formula_moiety         ' C22 H50 Cl2 N5 Nb1 Si3 '
_chemical_formula_sum            'C22 H50 Cl2 N5 Nb Si3'
_chemical_formula_weight         632.75
_chemical_name_systematic
;
 [Nb(NBu-t)Cl2(py){eta2-N(SiMe3)CH2CH2N(H)CH2CH2(SiMe3)2}]
;
_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   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 104.989(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0658(11)
_cell_length_b                   25.1387(24)
_cell_length_c                   15.1849(15)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      20.2
_cell_measurement_theta_min      13.1
_cell_volume                     3342.9(6)
_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'
_diffrn_measurement_method
; Scan width (omega) = 1.07 - 1.53, scan ratio 2theta:omega = 1.00
  I(Net) and sigma(I) from profile fitting (Clegg, 1981)
;
_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  0.03
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6412
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        'variation +/- 5.6'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.63
_exptl_absorpt_correction_T_max  0.5866
_exptl_absorpt_correction_T_min  0.4941
_exptl_absorpt_correction_type   'psi scans'
_exptl_absorpt_process_details
;
    Psi Scan Reflections used      

    H   K   L   2Theta   Chi   Imin/Imax
   -1  -4  -1     8.8   -75.7    0.880
    1   5   0     9.3    83.6    0.915
   -1  -6  -2    12.7   -71.2    0.925
   -2  -6  -1    14.2   -74.4    0.907
   -2  -9  -1    18.0   -85.7    0.838
   -3 -10  -1    22.1   -78.7    0.891
   -3 -12  -1    24.7   -83.8    0.897
   -2 -15  -2    27.3   -81.5    0.785
   -4 -17   2    33.3   -74.2    0.886
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.26
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.660
_exptl_crystal_size_mid          0.540
_exptl_crystal_size_min          0.420
_refine_diff_density_max         1.49
_refine_diff_density_min         -0.86
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.272
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5864
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_obs          0.0425
_refine_ls_shift/esd_max         0.03091
_refine_ls_structure_factor_coef F**2
_refine_ls_weighting_scheme      'Chebychev polynomial'
_refine_ls_wR_factor_all         0.0479
_refine_ls_wR_factor_obs         0.0430
_reflns_d_resolution_high        0.840
_reflns_d_resolution_low         8.111
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              29
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_observed          5000
_reflns_number_total             5864
_reflns_observed_criterion       >2.00\s(I)
_cod_data_source_file            ic991014c_1.cif
_cod_data_source_block           COMPOUND_3
_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'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        3342.9(5)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C22 H50 Cl2 N5 Nb1 Si3 '
_cod_database_code               4320905