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_4112718
_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            'C76 H122 O2 Si6 Y4'
_chemical_formula_weight         1591.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           52
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0952(8)
_cell_length_b                   25.5168(16)
_cell_length_c                   26.5227(16)
_cell_measurement_temperature    203(1)
_cell_volume                     8185.7(9)
_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 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0806
_diffrn_reflns_av_sigmaI/netI    0.0941
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            48154
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    2.936
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_description       block
_exptl_crystal_F_000             3336
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         9680
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.095
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                5378
_reflns_number_total             9680
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja047889urom20040413_031950.cif
_cod_data_source_block           5
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