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_4110671
_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            'C60 H108 O2 Si4 Y4'
_chemical_formula_weight         1329.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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                 103.3590(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2965(6)
_cell_length_b                   27.6752(14)
_cell_length_c                   19.0564(9)
_cell_measurement_temperature    163(2)
_cell_volume                     6822.7(6)
_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 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0537
_diffrn_reflns_av_sigmaI/netI    0.1273
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42590
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    3.474
_exptl_absorpt_correction_T_max  0.7226
_exptl_absorpt_correction_T_min  0.2755
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       plate
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.777
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         15380
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.777
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0185P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0614
_reflns_number_gt                8480
_reflns_number_total             15380
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja062348lsi20060517_113830.cif
_cod_data_source_block           2a
_cod_database_code               4110671