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_4069056
_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         '2(C39 H56 F6 N3 O2 Si V) C7 '
_chemical_formula_sum            'C85 H112 F12 N6 O4 Si2 V2'
_chemical_formula_weight         1667.89
_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'
_cell_angle_alpha                64.162(2)
_cell_angle_beta                 77.042(2)
_cell_angle_gamma                77.020(2)
_cell_formula_units_Z            1
_cell_length_a                   11.7792(10)
_cell_length_b                   14.5592(12)
_cell_length_c                   16.3464(14)
_cell_measurement_reflns_used    6779
_cell_measurement_temperature    193.1
_cell_measurement_theta_max      24.4
_cell_measurement_theta_min      3.0
_cell_volume                     2433.0(4)
_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  0.116
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18506
_diffrn_reflns_theta_full        24.41
_diffrn_reflns_theta_max         24.41
_exptl_absorpt_coefficient_mu    0.285
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             878.00
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.57
_refine_diff_density_min         -0.31
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     545
_refine_ls_number_reflns         2629
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
    Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
    4.2588    0.5646    3.2763
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                2582
_reflns_number_total             7952
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om8012234_si_003.cif
_cod_data_source_block           '_zhangwj-monoalkyl-4th'
_cod_original_formula_sum        'C85 H112 F12 N6 O4 Si2 V2 '
_cod_database_code               4069056