Synthesis of (Adamantylimido)vanadium(V) Dimethyl Complex Containing (2-Anilidomethyl)pyridine Ligand and Selected Reactions: Exploring the Oxidation State of the Catalytically Active Species in Ethylene Dimerization
Nomura, Kotohiro; Mitsudome, Takato; Igarashi, Atsushi; Nagai, Go; Tsutsumi, Ken; Ina, Toshiaki; Omiya, Takuya; Takaya, Hikaru; Yamazoe, Seiji; Organometallics 36 (2017) 530–; doi:10.1021/acs.organomet.6b00727

data_4086942
_publ_section_title
;
 Synthesis of (Adamantylimido)vanadium(V) Dimethyl Complex Containing
 (2-Anilidomethyl)pyridine Ligand and Selected Reactions: Exploring the
 Oxidation State of the Catalytically Active Species in Ethylene
 Dimerization
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              530
_journal_paper_doi               10.1021/acs.organomet.6b00727
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C26 H36 N3 V'
_chemical_formula_sum            'C26 H36 N3 V'
_chemical_formula_weight         441.53
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 116.714(14)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   18.883(19)
_cell_length_b                   14.196(13)
_cell_length_c                   20.00(2)
_cell_measurement_reflns_used    12128
_cell_measurement_temperature    273
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.59
_cell_volume                     4789(8)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r15'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r15'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      273
_diffrn_detector_area_resol_mean 13.653
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            49795
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.431
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       acicular
_exptl_crystal_F_000             1888.00
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.500
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_number_parameters     980
_refine_ls_number_reflns         10970
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0437P)^2^+2.0968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1380
_reflns_number_gt                9001
_reflns_number_total             10970
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om6b00727_si_002.cif
_cod_data_source_block           complex2a
_cod_depositor_comments
'Adding full bibliography for 4086942--4086945.cif.'
_cod_database_code               4086942