Reaction of (Bisimido)niobium(V) Complexes with Organic Azides: [3 + 2] Cycloaddition and Reversible Cleavage of β-Diketiminato Ligands Involving Nitrene Transfer.
Obenhuber, Andreas H.; Gianetti, Thomas L.; Berrebi, Xavier; Bergman, Robert G.; Arnold, John; Journal of the American Chemical Society 136 (2014) 2994–; doi:10.1021/ja413194z

data_4120632
_publ_section_title
;
 Reaction of (Bisimido)niobium(V) Complexes with Organic Azides: [3 + 2]
 Cycloaddition and Reversible Cleavage of \b-Diketiminato Ligands
 Involving Nitrene Transfer.
;
_journal_issue                   8
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2994
_journal_paper_doi               10.1021/ja413194z
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C37 H59 N4 Nb'
_chemical_formula_sum            'C37 H59 N4 Nb'
_chemical_formula_weight         652.79
_chemical_name_common            'Complex 6'
_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
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                105.313(2)
_cell_angle_beta                 102.083(2)
_cell_angle_gamma                98.673(2)
_cell_formula_units_Z            4
_cell_length_a                   11.1687(4)
_cell_length_b                   17.7140(6)
_cell_length_c                   19.7346(7)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    76(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      2.34
_cell_volume                     3593.3(2)
_computing_cell_refinement       'Bruker APEX2 v.2011.4'
_computing_data_collection       'Bruker APEX2 v.2011.4'
_computing_data_reduction        'Bruker APEX2 v.2011.4'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      76(2)
_diffrn_detector_area_resol_mean 8.336
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            57553
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.51
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.364
_exptl_absorpt_correction_T_max  0.9715
_exptl_absorpt_correction_T_min  0.9474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rode
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         13252
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0203P)^2^+4.3415P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0732
_reflns_number_gt                11230
_reflns_number_total             13252
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja413194z_si_003.cif
_cod_data_source_block           (5)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4120632