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_4069054
_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         'C32 H44 Cl2 N3 O V '
_chemical_formula_sum            'C32 H44 Cl2 N3 O V'
_chemical_formula_weight         608.57
_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                102.2975(17)
_cell_angle_beta                 91.9098(13)
_cell_angle_gamma                114.2485(15)
_cell_formula_units_Z            2
_cell_length_a                   10.1796(4)
_cell_length_b                   10.6325(5)
_cell_length_c                   17.0560(6)
_cell_measurement_reflns_used    12835
_cell_measurement_temperature    193.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.1
_cell_volume                     1629.37(12)
_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  0.028
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16190
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.722
_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    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             644.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.63
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     414
_refine_ls_number_reflns         5592
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[0.0103Fo^2^ + 1.0000\s(Fo^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1118
_reflns_number_gt                5558
_reflns_number_total             7409
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om8012234_si_003.cif
_cod_data_source_block           '_zhangwj-l3-ad-dichloro'
_cod_original_cell_volume        1629.37(10)
_cod_original_formula_sum        'C32 H44 Cl2 N3 O V '
_cod_database_code               4069054