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_4315432
_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         C16H46N8O2Nb2
_chemical_formula_sum            'C16 H46 N8 Nb2 O2'
_chemical_formula_weight         568.40
_chemical_name_common            'Niobium dimer'
_chemical_name_systematic
; 
Tantalum dimer 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.856(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.410(11)
_cell_length_b                   13.784(13)
_cell_length_c                   8.645(8)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.48
_cell_measurement_theta_min      2.39
_cell_volume                     1294(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1588
_diffrn_reflns_av_sigmaI/netI    0.0819
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4900
_diffrn_reflns_theta_full        22.48
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.910
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.935
_refine_diff_density_min         -1.497
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         894
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.257
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0750
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+26.2103P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1811
_refine_ls_wR_factor_ref         0.1812
_reflns_number_gt                890
_reflns_number_total             894
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901889m_si_002_2.cif
_cod_data_source_block           a
_cod_depositor_comments
;
 Removing the _chemical_melting_point data item since it contained the
 _chemical_formula_sum data item value and not the melting temperature.

 Antanas Vaitkus,
 2017-09-27

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_cell_measurement_temperature' value '173(2)K' was changed to
'173(2)' - the value should be numeric and without a unit
designator.

'_diffrn_ambient_temperature' value '173(2)k' was
changed to '173(2)' - the value should be numeric and without a unit
designator.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_formula_sum        C16H46N8O2Nb2
_cod_database_code               4315432