Well-Defined Vanadium Organoazide Complexes and Their Conversion to Terminal Vanadium Imides: Structural Snapshots and Evidence for a Nitrene Capture Mechanism
W. Hill Harman; Michael F. Lichterman; Nicholas A. Piro; Christopher J. Chang; Inorganic Chemistry 51 (2012) 10037–10042; doi:10.1021/ic301673g

data_4330421
_publ_section_title
;
 Well-Defined Vanadium Organoazide Complexes and Their Conversion to
 Terminal Vanadium Imides: Structural Snapshots and Evidence for a Nitrene
 Capture Mechanism
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10037
_journal_page_last               10042
_journal_paper_doi               10.1021/ic301673g
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C49 H52 N5 V'
_chemical_formula_sum            'C49 H52 N5 V'
_chemical_formula_weight         761.90
_chemical_name_common            (tpaMes)V(NpTol)
_chemical_name_systematic        (tpaMes)V(NpTol)
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 93.621(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1269(4)
_cell_length_b                   10.7324(3)
_cell_length_c                   21.7556(5)
_cell_measurement_reflns_used    8301
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.5
_cell_measurement_theta_min      2.6
_cell_volume                     3990.97(17)
_computing_cell_refinement       'Bruker APEX2 v. 2009.3'
_computing_data_collection       'Bruker APEX2 v. 2009.3'
_computing_data_reduction        'Bruker APEX2 v. 2009.3'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'HELIOS multilayer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0723
_diffrn_reflns_av_sigmaI/netI    0.0736
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36237
_diffrn_reflns_theta_full        66.75
_diffrn_reflns_theta_max         66.75
_diffrn_reflns_theta_min         2.58
_diffrn_source                   'microfocus rotating anode'
_exptl_absorpt_coefficient_mu    2.386
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       plate
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         6993
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+1.6072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                4769
_reflns_number_total             6993
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301673g_si_001_4.cif
_cod_data_source_block           3c
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4330421