1,2-C−H Activation of Benzene Promoted by (Arylimido)vanadium(V)-Alkylidene Complexes: Isolation of the Alkylidene, Benzyne Complexes
Zhang, Shu; Tamm, Matthias; Nomura, Kotohiro; Organometallics 30 (2011) 2712–; doi:10.1021/om200086n

data_4064407
_publ_section_title
;
 1,2-C&#x2212;H Activation of Benzene Promoted by
 (Arylimido)vanadium(V)-Alkylidene Complexes: Isolation of the Alkylidene,
 Benzyne Complexes
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2712
_journal_paper_doi               10.1021/om200086n
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C35 H45 Cl2 N4 V '
_chemical_formula_sum            'C35 H45 Cl2 N4 V'
_chemical_formula_weight         643.61
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 102.1747(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.0737(3)
_cell_length_b                   19.7240(5)
_cell_length_c                   16.2785(3)
_cell_measurement_reflns_used    22086
_cell_measurement_temperature    153.1
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.0
_cell_volume                     3475.55(14)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      153.1
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28231
_diffrn_reflns_theta_full        25.32
_diffrn_reflns_theta_max         25.32
_exptl_absorpt_coefficient_mu    0.467
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1360.00
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.29
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     380
_refine_ls_number_reflns         6321
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0404P)^2^+1.6956P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0850
_reflns_number_gt                5681
_reflns_number_total             6321
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om200086n_si_002.cif
_cod_data_source_block           '_V(NAr)Cl2(ImDIPP-N)zs'
_cod_original_cell_volume        3475.56(14)
_cod_original_formula_sum        'C35 H45 Cl2 N4 V '
_cod_database_code               4064407