Synthesis of (1-Adamantylimido)vanadium(V)-alkyl Complexes Containing a Chelate Alkoxo(imino)pyridine Ligand, and Reactions with Alcohols (ROH) That Proceed via Intermediates Formed by Coordination of ROH
Zhang, Wenjuan; Katao, Shohei; Sun, Wen-Hua; Nomura, Kotohiro; Organometallics 28 (2009) 1558–; doi:10.1021/om8012234

data_4069055
_publ_section_title
;
 Synthesis of (1-Adamantylimido)vanadium(V)-alkyl Complexes Containing a
 Chelate Alkoxo(imino)pyridine Ligand, and Reactions with Alcohols (ROH)
 That Proceed via Intermediates Formed by Coordination of ROH
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1558
_journal_paper_doi               10.1021/om8012234
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C60 H84 N5 O2 Si V '
_chemical_formula_sum            'C60 H84 N5 O2 Si V'
_chemical_formula_weight         986.38
_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                 97.306(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   16.5172(16)
_cell_length_b                   16.9839(15)
_cell_length_c                   21.2017(18)
_cell_measurement_reflns_used    11209
_cell_measurement_temperature    193.1
_cell_measurement_theta_max      23.2
_cell_measurement_theta_min      3.0
_cell_volume                     5899.4(9)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.168
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38733
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_exptl_absorpt_coefficient_mu    0.231
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2128.00
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.20
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     696
_refine_ls_number_reflns         2250
_refine_ls_R_factor_gt           0.0681
_refine_ls_shift/su_max          0.0003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0047Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1715
_reflns_number_gt                2220
_reflns_number_total             8407
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om8012234_si_003.cif
_cod_data_source_block           '_zhangwj-monoalkyl'
_cod_original_formula_sum        'C60 H84 N5 O2 Si V '
_cod_database_code               4069055