Synthesis of (Imido)vanadium(V) Alkyl and Alkylidene Complexes Containing Imidazolidin-2-iminato Ligands: Effect of Imido Ligand on ROMP and 1,2-C‒H Bond Activation of Benzene
Nomura, Kotohiro; Bahuleyan, Bijal Kottukkal; Tsutsumi, Ken; Igarashi, Atsushi; Organometallics 33 (2014) 6682–; doi:10.1021/om500986m

data_4084769
_publ_section_title
;
 Synthesis of (Imido)vanadium(V) Alkyl and Alkylidene Complexes Containing
 Imidazolidin-2-iminato Ligands: Effect of Imido Ligand on ROMP and
 1,2-C--H Bond Activation of Benzene
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6682
_journal_paper_doi               10.1021/om500986m
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C45 H75 N4 Si2 V'
_chemical_formula_sum            'C45 H75 N4 Si2 V'
_chemical_formula_weight         779.23
_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
_cell_angle_alpha                85.3288(7)
_cell_angle_beta                 86.9167(7)
_cell_angle_gamma                72.4998(7)
_cell_formula_units_Z            2
_cell_length_a                   10.8115(2)
_cell_length_b                   12.2653(3)
_cell_length_c                   18.3622(4)
_cell_measurement_reflns_used    20862
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.00
_cell_volume                     2313.43(9)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0159
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23220
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.299
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             848.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.330
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     483
_refine_ls_number_reflns         10558
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0658P)^2^+0.5107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1122
_reflns_number_gt                9653
_reflns_number_total             10558
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om500986m_si_003.cif
_cod_data_source_block           AdV(CH2TMS)2(iPrPh)2N
_cod_depositor_comments          'Adding full bibliography for 4084769.cif.'
_cod_original_cell_volume        2313.43(8)
_cod_database_code               4084769