Hydrogenation of Carbon Monoxide by Tetranuclear Rare Earth Metal Polyhydrido Complexes. Selective Formation of Ethylene and Isolation of Well-Defined Polyoxo Rare Earth Metal Clusters
Takanori Shima; Zhaomin Hou; Journal of the American Chemical Society 128 (2006) 8124–8125; doi:10.1021/ja062348l

data_4110672
_publ_section_title
;
 Hydrogenation of Carbon Monoxide by Tetranuclear Rare Earth Metal
 Polyhydrido Complexes. Selective Formation of Ethylene and Isolation of
 Well-Defined Polyoxo Rare Earth Metal Clusters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8124
_journal_page_last               8125
_journal_paper_doi               10.1021/ja062348l
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C59 H104 O3 Si4 Y4'
_chemical_formula_weight         1329.42
_chemical_name_systematic
; 
 ? 
;
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_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.1600(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.2952(11)
_cell_length_b                   14.6232(8)
_cell_length_c                   24.9276(14)
_cell_measurement_temperature    163(2)
_cell_volume                     6899.2(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_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  0.0678
_diffrn_reflns_av_sigmaI/netI    0.1353
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            42233
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    3.437
_exptl_absorpt_correction_T_max  0.7250
_exptl_absorpt_correction_T_min  0.2783
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       block
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.502
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.890
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         15406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.890
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1188
_reflns_number_gt                8270
_reflns_number_total             15406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja062348lsi20060517_113845.cif
_cod_data_source_block           4
_cod_database_code               4110672