Synthesis of (Adamantylmido)vanadium(V)-Alkyl, Alkylidene Complex Trapped with PMe3: Reactions of the Alkylidene Complexes with Phenols
Hatagami, Kohei; Nomura, Kotohiro; Organometallics 33 (2014) 6585–; doi:10.1021/om500923y

data_4084667
_publ_section_title
;
 Synthesis of (Adamantylmido)vanadium(V)-Alkyl, Alkylidene Complex Trapped
 with PMe3: Reactions of the Alkylidene Complexes with Phenols
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6585
_journal_paper_doi               10.1021/om500923y
_journal_volume                  33
_journal_year                    2014
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C24 H54 N P2 Si2 V'
_chemical_formula_sum            'C24 H54 N P2 Si2 V'
_chemical_formula_weight         525.76
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                101.924(3)
_cell_angle_beta                 101.373(7)
_cell_angle_gamma                105.836(13)
_cell_formula_units_Z            2
_cell_length_a                   10.339(3)
_cell_length_b                   10.355(3)
_cell_length_c                   17.415(5)
_cell_measurement_reflns_used    4812
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.70
_cell_volume                     1690.1(9)
_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    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 6.827
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0341
_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       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17839
_diffrn_reflns_theta_full        27.62
_diffrn_reflns_theta_max         27.62
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.469
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.033
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             572.00
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.880
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     284
_refine_ls_number_reflns         7765
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0944P)^2^+2.9505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1813
_reflns_number_gt                6564
_reflns_number_total             7765
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om500923y_si_004.cif
_cod_data_source_block           SX150a
_cod_depositor_comments
'Adding full bibliography for 4084667--4084668.cif.'
_cod_database_code               4084667