Formation of Aminoxy and Oxo Complexes from the Reaction of Nb(NMe2)5 with O2 and the Crystal Structure of Nb(NEt2)5
Shu-Jian Chen; Jian Zhang; Xianghua Yu; Xianhui Bu; Xue-Tai Chen; Zi-Ling Xue; Inorganic Chemistry 49 (2010) 4017–4022; doi:10.1021/ic901889m

data_4315433
_publ_section_title
;
 Formation of Aminoxy and Oxo Complexes from the Reaction of Nb(NMe2)5
 with O2 and the Crystal Structure of Nb(NEt2)5
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4017
_journal_page_last               4022
_journal_paper_doi               10.1021/ic901889m
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         C20H50N5Nb
_chemical_formula_sum            'C20 H50 N5 Nb'
_chemical_formula_weight         453.56
_chemical_name_common            'pentakis(diethylamido) Niobium '
_chemical_name_systematic
; 
pentakis(diethylamido) Niobium 
;
_space_group_IT_number           1
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.456(13)
_cell_angle_beta                 83.912(13)
_cell_angle_gamma                65.483(12)
_cell_formula_units_Z            3
_cell_length_a                   9.293(10)
_cell_length_b                   10.103(11)
_cell_length_c                   22.35(2)
_cell_measurement_temperature    173(2)
_cell_volume                     1890(3)
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_collection       'SMART, Bruker (2000)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL, Bruker (2000)'
_computing_publication_material  'SHELXTL, Bruker (2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0851
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            18123
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         0.92
_exptl_absorpt_coefficient_mu    0.490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             738
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         5.677
_refine_diff_density_min         -1.390
_refine_diff_density_rms         0.214
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.44(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         14213
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0774
_refine_ls_shift/su_max          0.461
_refine_ls_shift/su_mean         0.040
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1394P)^2^+2.9529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1973
_refine_ls_wR_factor_ref         0.2327
_reflns_number_gt                10643
_reflns_number_total             14213
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901889m_si_002_3.cif
_cod_data_source_block           nemo2_p1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4315433