Mononuclear Niobium Imido and Oxo Complexes Supported by N,N'-Bis(trimethylsilyl)benzamidinate Ligands. X-ray Structures of [Nb(NBut){PhC(NSiMe3)2}Cl2(py)] and [Nb(O){(4-C6H4Me)C(NSiMe3)2}2Cl]
Peter J. Stewart; Alexander J. Blake; Philip Mountford; Inorganic Chemistry 36 (1997) 1982–1986; doi:10.1021/ic961391e

data_4323396
_publ_contact_author
;
 Dr P Mountford
 Department of Chemistry
 University of Nottingham
 Nottingham
 NG7 2RD
 UK
;
_publ_contact_author_email       Philip.Mountford@nott.ac.uk
_publ_contact_author_fax         '+44 115 951 3563'
_publ_contact_author_phone       '+44 115 951 3513'
_publ_section_title
;
 Mononuclear Niobium Imido and Oxo Complexes Supported by
 N,N'-Bis(trimethylsilyl)benzamidinate Ligands. X-ray Structures of
 [Nb(NBut){PhC(NSiMe3)2}Cl2(py)] and [Nb(O){(4-C6H4Me)C(NSiMe3)2}2Cl]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1982
_journal_page_last               1986
_journal_paper_doi               10.1021/ic961391e
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source
;
 Li[4-Me-C6H4C(NSiMe3)2] + [Nb(Nbu-t)Cl3(py)2]
 recrystallise from hexane
;
_chemical_formula_moiety         ' C22 H37 Nb1 N4 Si2 Cl2 , 0.25(C6 H14) '
_chemical_formula_sum            'C23.5 H40.5 Cl2 N4 Nb Si2'
_chemical_formula_weight         599.09
_chemical_name_systematic
;
 [Nb(NBu-t){PhC(NSiMe3)2}Cl2(py)] . 0.25(C6H14)
;
_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   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                91.368(15)
_cell_angle_beta                 95.509(22)
_cell_angle_gamma                93.025(19)
_cell_formula_units_Z            4.0
_cell_length_a                   10.972(3)
_cell_length_b                   17.100(4)
_cell_length_c                   17.777(3)
_cell_measurement_reflns_used    31
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      17.0
_cell_measurement_theta_min      14.2
_cell_volume                     3313.9(13)
_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 (Watkin et al, 1996)'
_computing_structure_refinement  'CRYSTALS (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       \q/\w
_diffrn_radiation_detector       'NaI(Tl) scintillation counter'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  90.0
_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       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11217
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        6.8
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  0.5011
_exptl_absorpt_correction_T_min  0.4414
_exptl_absorpt_correction_type   psi-scans
_exptl_absorpt_process_details
;
  7 Psi Scan Reflections used    Mu * R = 0.48  
    H   K   L   2Theta   Chi   Imin/Imax
    0   4  -2    10.5   -78.9    0.929
    0   4  -2    10.5   -78.9    0.934
    1   7   0    17.4   -60.1    0.887
    0  -7   5    20.1    72.2    0.876
   -1  12   0    29.0   -71.1    0.934
   -2  14   3    35.1   -60.1    0.913
    2 -15   4    37.9    85.4    0.925
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.20
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             1250
_exptl_crystal_size_max          0.750
_exptl_crystal_size_mid          0.675
_exptl_crystal_size_min          0.600
_refine_diff_density_max         0.18
_refine_diff_density_min         -0.19
_refine_ls_extinction_coef       41.2(159)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_obs   0.9635
_refine_ls_hydrogen_treatment
;
 H atoms placed geometrically and refined with riding model
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         10313
_refine_ls_number_restraints     14
_refine_ls_R_factor_obs          0.0352
_refine_ls_shift/esd_max         0.580119
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
;
 Chebychev polynomial (Carruthers & Watkin, 1979)
;
_refine_ls_wR_factor_obs         0.0407
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              20
_reflns_limit_k_min              -20
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_observed          10313
_reflns_number_total             11217
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            ic961391e_2.cif
_cod_data_source_block           COMPOUND2_HEXANE_SOLVATE
_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        3313.9(10)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C23.5 H40.5 Nb1 N4 Si2 Cl2 '
_cod_database_code               4323396