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_4084668
_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_formula_moiety         'C28 H52 N O P2 Si V'
_chemical_formula_sum            'C28 H52 N O P2 Si V'
_chemical_formula_weight         559.70
_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                99.891(12)
_cell_angle_beta                 90.355(6)
_cell_angle_gamma                103.274(16)
_cell_formula_units_Z            4
_cell_length_a                   12.461(4)
_cell_length_b                   13.957(5)
_cell_length_c                   19.235(5)
_cell_measurement_reflns_used    8801
_cell_measurement_temperature    273
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.05
_cell_volume                     3203.9(18)
_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    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      273
_diffrn_detector_area_resol_mean 13.653
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.1024
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32271
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.466
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1208.00
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
;
_refine_diff_density_max         1.420
_refine_diff_density_min         -0.960
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     621
_refine_ls_number_reflns         14537
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0848
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0943P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2319
_reflns_number_gt                8330
_reflns_number_total             14537
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om500923y_si_004.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4084667--4084668.cif.'
_cod_original_cell_volume        3203.8(16)
_cod_database_code               4084668