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_4104041
_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_sum            'C174 H242 K2 O28 Ta4'
_chemical_formula_weight         3583.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.080(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.660(6)
_cell_length_b                   26.919(8)
_cell_length_c                   18.596(6)
_cell_measurement_reflns_used    22777
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0267
_cell_volume                     8536(5)
_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      173(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Saturn70 CCD (4x4 bin mode)'
_diffrn_measurement_method       dtintegrate.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_sigmaI/netI    0.0931
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            52948
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    2.670
_exptl_absorpt_correction_T_max  0.7761
_exptl_absorpt_correction_T_min  0.6902
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3680
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.432
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.261
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     895
_refine_ls_number_reflns         14722
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.261
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_gt           0.1003
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+74.8144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1868
_refine_ls_wR_factor_ref         0.1975
_reflns_number_gt                12593
_reflns_number_total             14722
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9007276_si_001.cif
_cod_data_source_block           '[{(OOO)Ta}4(C6O6)H2(THF)2{K(DME)}]4THF'
_cod_database_code               4104041