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_4330418
_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 O V'
_chemical_formula_sum            'C52.5 H56 N7 O V'
_chemical_formula_weight         851.98
_chemical_name_common            tpaMesV(N3Ar)
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.938(4)
_cell_angle_beta                 99.085(4)
_cell_angle_gamma                109.141(4)
_cell_formula_units_Z            4
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_cell_length_b                   19.227(5)
_cell_length_c                   19.880(5)
_cell_measurement_reflns_used    4743
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      21.6
_cell_measurement_theta_min      2.3
_cell_volume                     4482.8(19)
_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    Mercury
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      105(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-I 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  0.0631
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_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34286
_diffrn_reflns_theta_full        25.47
_diffrn_reflns_theta_max         25.47
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.8060
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       block
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_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1111
_refine_ls_number_reflns         16221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1758
_refine_ls_R_factor_gt           0.0754
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1036P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.2133
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301673g_si_001_1.cif
_cod_data_source_block           2a
_cod_original_cell_volume        4483(2)
_cod_original_formula_sum        'C52.50 H56 N7 O V'
_cod_database_code               4330418