Hydrogenation of Carbon Dioxide and Aryl Isocyanates by a Tetranuclear Tetrahydrido Yttrium Complex. Isolation, Structures, and CO2 Insertion Reactions of Methylene Diolate and μ3-Oxo Yttrium Complexes
Olivier Tardif; Daisuke Hashizume; Zhaomin Hou; Journal of the American Chemical Society 126 (2004) 8080–8081; doi:10.1021/ja047889u

data_4112717
_publ_section_title
;
 Hydrogenation of Carbon Dioxide and Aryl Isocyanates by a Tetranuclear
 Tetrahydrido Yttrium Complex. Isolation, Structures, and CO2 Insertion
 Reactions of Methylene Diolate and \m3-Oxo Yttrium Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8080
_journal_page_last               8081
_journal_paper_doi               10.1021/ja047889u
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C74 H120 O6 Si6 Y4'
_chemical_formula_weight         1629.88
_chemical_name_systematic
; 
 ? 
;
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_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.319(2)
_cell_angle_beta                 92.998(2)
_cell_angle_gamma                92.442(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2223(14)
_cell_length_b                   13.9952(16)
_cell_length_c                   24.050(3)
_cell_measurement_temperature    203(1)
_cell_volume                     4069.7(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(1)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0856
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            24631
_diffrn_reflns_theta_full        27.03
_diffrn_reflns_theta_max         27.03
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    2.957
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       bar
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.147
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         17165
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.386
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1192
_reflns_number_gt                10898
_reflns_number_total             17165
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja047889urom20040413_031930.cif
_cod_data_source_block           4
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