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_4086945
_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         'C29 H42 N3 O V'
_chemical_formula_sum            'C29 H42 N3 O V'
_chemical_formula_weight         499.61
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 97.308(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   10.439(7)
_cell_length_b                   15.275(10)
_cell_length_c                   17.444(11)
_cell_measurement_reflns_used    8067
_cell_measurement_temperature    273
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.54
_cell_volume                     2759(3)
_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    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      273
_diffrn_detector_area_resol_mean 13.653
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0346
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28471
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.384
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1072.00
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.230
_refine_diff_density_max         1.070
_refine_diff_density_min         -0.590
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     307
_refine_ls_number_reflns         6293
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1028P)^2^+1.2910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1615
_reflns_number_gt                5263
_reflns_number_total             6293
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om6b00727_si_002.cif
_cod_data_source_block           Complex3c
_cod_depositor_comments
'Adding full bibliography for 4086942--4086945.cif.'
_cod_database_code               4086945