Synthesis of Various (Arylimido)vanadium(V)−Methyl Complexes Containing Ketimide Ligands and Reactions with Alcohols, Thiols, and Borates: Implications for Unique Reactivity toward Alcohols
Yamada, Junji; Fujiki, Michiya; Nomura, Kotohiro; Organometallics 26 (2007) 2579–; doi:10.1021/om061121w

data_4072897
_publ_section_title
;
 Synthesis of Various (Arylimido)vanadium(V)&#x2212;Methyl Complexes
 Containing Ketimide Ligands and Reactions with Alcohols, Thiols, and
 Borates:&#x00A0; Implications for Unique Reactivity toward Alcohols
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2579
_journal_paper_doi               10.1021/om061121w
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C54 H53 B F20 N3 O V '
_chemical_formula_sum            'C54 H53 B F20 N3 O V'
_chemical_formula_weight         1201.75
_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'
_cell_angle_alpha                90.0000
_cell_angle_beta                 93.897(13)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.606(5)
_cell_length_b                   15.262(4)
_cell_length_c                   24.342(6)
_cell_measurement_reflns_used    34515
_cell_measurement_temperature    243.1
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.0
_cell_volume                     5784(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.039
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            53601
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.275
_exptl_absorpt_correction_T_max  0.886
_exptl_absorpt_correction_T_min  0.551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2456.00
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.88
_refine_diff_density_min         -0.38
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     802
_refine_ls_number_reflns         7733
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.0015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0039Fo^2^ + 1.0100\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1632
_reflns_number_gt                7671
_reflns_number_total             13206
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om061121wsi20061211_072857.cif
_cod_data_source_block           '_Me2NV(NCtBu2)2(thf)2-B(C6'
_cod_original_formula_sum        'C54 H53 B F20 N3 O V '
_cod_database_code               4072897