Reductive Coupling of Six Carbon Monoxides by a Ditantalum Hydride Complex
Takahito Watanabe; Yutaka Ishida; Tsukasa Matsuo; Hiroyuki Kawaguchi; Journal of the American Chemical Society 131 (2009) 3474–3475; doi:10.1021/ja9007276

data_4104042
_publ_contact_author_email       hkawa@chem.titech.ac.jp
_publ_contact_author_name        'Hioryuki Kawaguchi'
_publ_section_title
;
 Reductive Coupling of Six Carbon Monoxides by a Ditantalum Hydride
 Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3474
_journal_page_last               3475
_journal_paper_doi               10.1021/ja9007276
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C158 H204 O22 Ta4''C4 H8 O''C4 H8 O'
_chemical_formula_sum            'C166 H220 O24 Ta4'
_chemical_formula_weight         3323.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                115.639(3)
_cell_angle_beta                 106.946(4)
_cell_angle_gamma                97.7005(16)
_cell_formula_units_Z            1
_cell_length_a                   13.695(5)
_cell_length_b                   18.865(7)
_cell_length_c                   19.053(8)
_cell_measurement_reflns_used    10838
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0957
_cell_volume                     4047(3)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 14.6199
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Mercury CCD (2x2 bin mode)'
_diffrn_measurement_method       dtintegrate.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0564
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32107
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    2.758
_exptl_absorpt_correction_T_max  0.8095
_exptl_absorpt_correction_T_min  0.6666
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         7.671
_refine_diff_density_min         -2.677
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    calcd
_refine_ls_matrix_type           full
_refine_ls_number_parameters     863
_refine_ls_number_reflns         17740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0754
_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^)+(0.1196P)^2^+30.3638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1954
_refine_ls_wR_factor_ref         0.2089
_reflns_number_gt                13766
_reflns_number_total             17740
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9007276_si_002.cif
_cod_data_source_block
'[(tBu-L)Ta(THF)]4[OC=C(O)C(O)=C(O)C(O)=CO](THF)2'
_cod_database_code               4104042