Silicon-Bridged Tetramethylcyclopentadienyl−Phenoxy Complexes of Tantalum: Preparation and Alkylation of Et2Si(η5-C5Me4)(3-tBu-5-Me-2-C6H2O)TaCl3and Generation of Its Cationic Complex
Senda, Taichi; Hanaoka, Hidenori; Oda, Yoshiaki; Tsurugi, Hayato; Mashima, Kazushi; Organometallics 29 (2010) 2080–; doi:10.1021/om100042t

data_4065634
_publ_section_title
;
 Silicon-Bridged Tetramethylcyclopentadienyl&#x2212;Phenoxy Complexes of
 Tantalum: Preparation and Alkylation of
 Et2Si(\h5-C5Me4)(3-tBu-5-Me-2-C6H2O)TaCl3and Generation of Its Cationic
 Complex
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2080
_journal_paper_doi               10.1021/om100042t
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C24 H36 Cl3 O Si Ta'
_chemical_formula_sum            'C24 H36 Cl3 O Si Ta'
_chemical_formula_weight         655.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.316(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6996(19)
_cell_length_b                   15.375(3)
_cell_length_c                   17.381(4)
_cell_measurement_reflns_used    7289
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_cell_volume                     2576.3(9)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    Oretp-3
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18691
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.27
_exptl_absorpt_coefficient_mu    4.638
_exptl_absorpt_correction_T_max  0.6541
_exptl_absorpt_correction_T_min  0.2584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.691
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.747
_refine_diff_density_min         -1.767
_refine_diff_density_rms         0.423
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.243
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5778
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.243
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+2.3888P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.1014
_reflns_number_gt                5088
_reflns_number_total             5778
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100042t_si_002.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        2576.4(9)
_cod_database_code               4065634