Carbon versus Silicon Bridges. Synthesis of a New Versatile Ligand and Its Applications in Organolanthanide Chemistry
Wang, Shaowu; Yang, Qingchuan; Mak, Thomas C. W.; Xie, Zuowei; Organometallics 19 (2000) 334–; doi:10.1021/om990648o

data_4077668
_publ_section_title
;
 Carbon versus Silicon Bridges. Synthesis of a New Versatile Ligand and
 Its Applications in Organolanthanide Chemistry
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              334
_journal_paper_doi               10.1021/om990648o
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C47 H82 B20 Li O6 Yb'
_chemical_formula_weight         1139.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.716(3)
_cell_length_b                   21.471(4)
_cell_length_c                   22.011(4)
_cell_measurement_temperature    293(2)
_cell_volume                     6010(2)
_computing_cell_refinement       'BIOTEX Rigaku'
_computing_data_collection       'RAXIS Rigaku'
_computing_data_reduction        'BIOTEX Rigaku'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'IP Rigaku'
_diffrn_measurement_method       IP
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotation anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_sigmaI/netI    0.0976
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6530
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    1.599
_exptl_absorpt_correction_T_max  1.539
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   abscor
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2340
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.51(3)
_refine_ls_extinction_coef       0.00000(6)
_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   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         5858
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.756
_refine_ls_shift/su_mean         0.034
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1477
_refine_ls_wR_factor_ref         0.1523
_reflns_number_gt                5260
_reflns_number_total             5858
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om990648o.cif
_cod_data_source_block           compound_7
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4077668