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_4323395
_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
;
 reaction between [Nb(O)Cl3(thf)2] and 2 Li[MeC6H4C(NSiMe3)2] in thf
;
_chemical_formula_moiety         ' C28 H50 Nb1 O1 Cl1 N4 Si4 '
_chemical_formula_sum            'C28 H50 Cl N4 Nb O Si4'
_chemical_formula_weight         699.433
_chemical_name_systematic
;
 [Nb(O){(4-C6H4Me)C(NSiMe3)2}2Cl]
;
_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     SIR92
_cell_angle_alpha                100.65(6)
_cell_angle_beta                 93.92(6)
_cell_angle_gamma                106.90(6)
_cell_formula_units_Z            2.00
_cell_length_a                   10.573(9)
_cell_length_b                   11.173(8)
_cell_length_c                   17.028(14)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    220(1)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      13.5
_cell_volume                     1876(3)
_computing_cell_refinement       'STADI4 (STOE 1995a)'
_computing_data_collection       'STADI4 (STOE 1995a)'
_computing_data_reduction
;
X-RED (STOE, 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 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      220
_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  0.048
_diffrn_reflns_av_sigmaI/netI    0.08211
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6566
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        11.2
_diffrn_standards_interval_time  '60 minutes'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.739
_exptl_absorpt_correction_type   'psi scans'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.2384
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.50
_refine_diff_density_max         1.99
_refine_diff_density_min         -0.27
_refine_ls_abs_structure_Flack   0
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     'not required'
_refine_ls_goodness_of_fit_obs   1.3277
_refine_ls_hydrogen_treatment    'Riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         3769
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0574
_refine_ls_shift/esd_max         0.098971
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.0643
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_observed          3769
_reflns_number_total             5026
_reflns_observed_criterion       >2.00\s(I)
_cod_data_source_file            ic961391e_1.cif
_cod_data_source_block           COMPOUND4
_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:

'_refine_ls_weighting_scheme' value 'Unit weights' was changed to
'unit'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z 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        1875.4(3)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C28 H50 Nb1 O1 Cl1 N4 Si4 '
_cod_database_code               4323395