Synthesis and Structural Characterization of the First Lanthanide(II) Cuboidal Cluster. Unexpected C−O Activation by an Unchanged Ytterbium(II) Center
Clegg, William; Izod, Keith; Liddle, Stephen T.; O'Shaughness, Paul; Sheffield, Joanne M.; Organometallics 19 (2000) 2090–; doi:10.1021/om000057u

data_4077477
_publ_section_title
;
 Synthesis and Structural Characterization of the First Lanthanide(II)
 Cuboidal Cluster. Unexpected C&#x2212;O Activation by an Unchanged
 Ytterbium(II) Center
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2090
_journal_paper_doi               10.1021/om000057u
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C84 H164 O12 P4 Si8 Yb4'
_chemical_formula_weight         2406.91
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.323(4)
_cell_length_b                   20.323(4)
_cell_length_c                   12.743(3)
_cell_measurement_reflns_used    17711
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.75
_cell_volume                     5263.2(19)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14958
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.723
_exptl_absorpt_correction_T_max  0.3888
_exptl_absorpt_correction_T_min  0.2660
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.097
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.491(8)
_refine_ls_extinction_coef       0.00011(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         5129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0544
_reflns_number_gt                4806
_reflns_number_total             5129
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000057u.cif
_cod_data_source_block           ki47
_cod_original_cell_volume        5263.2(18)
_cod_original_sg_symbol_H-M      I-4
_cod_database_code               4077477