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_4330419
_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         'C3.5 H4, C49 H52 N7 V'
_chemical_formula_sum            'C52.5 H56 N7 V'
_chemical_formula_weight         836.00
_chemical_name_common            (tpaMes)V(N3pTol)
_chemical_name_systematic        (tpaMes)V(N3pTol)
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                98.969(4)
_cell_angle_beta                 98.736(3)
_cell_angle_gamma                108.891(3)
_cell_formula_units_Z            4
_cell_length_a                   12.9102(6)
_cell_length_b                   19.1239(10)
_cell_length_c                   19.6489(10)
_cell_measurement_reflns_used    9613
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.2
_cell_measurement_theta_min      2.5
_cell_volume                     4426.2(4)
_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-32
_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 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'HELIOS multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_sigmaI/netI    0.0971
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35432
_diffrn_reflns_theta_full        49.09
_diffrn_reflns_theta_max         49.09
_diffrn_reflns_theta_min         2.33
_diffrn_source                   'microfocus rotating anode'
_exptl_absorpt_coefficient_mu    2.206
_exptl_absorpt_correction_T_max  0.751
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       block
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1111
_refine_ls_number_reflns         8495
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1211
_refine_ls_R_factor_gt           0.0677
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+2.4514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1568
_reflns_number_gt                5213
_reflns_number_total             8495
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301673g_si_001_2.cif
_cod_data_source_block           2c
_cod_database_code               4330419