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_4104043
_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         'C150 H188 O20 Ta4''C5 H12'
_chemical_formula_sum            'C155 H200 O20 Ta4'
_chemical_formula_weight         3106.95
_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                80.559(4)
_cell_angle_beta                 78.017(4)
_cell_angle_gamma                73.103(3)
_cell_formula_units_Z            4
_cell_length_a                   20.306(2)
_cell_length_b                   24.091(3)
_cell_length_c                   34.887(4)
_cell_measurement_reflns_used    36160
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0043
_cell_volume                     15876(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, 1997)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 14.6199
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_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  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0806
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            127436
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    2.806
_exptl_absorpt_correction_T_max  0.8067
_exptl_absorpt_correction_T_min  0.6783
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             6328
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.490
_refine_diff_density_min         -1.436
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    calcd
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3191
_refine_ls_number_reflns         69785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0755P)^2^+122.0789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1623
_refine_ls_wR_factor_ref         0.1784
_reflns_number_gt                49912
_reflns_number_total             69785
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9007276_si_003.cif
_cod_data_source_block
'[(tBu-L)Ta(THF)]2[(tBu-L)Ta]2[OC=C(O)C(O)=C(O)C(O)=CO]pentane'
_cod_original_cell_volume        15875(3)
_cod_database_code               4104043