Dynamic Resolution of a Metallocene: Diastereoselective Assembly of an Early-Late Heterobimetallic Metal-Bridgedansa-Metallocene Opening a Route to Parallel Catalyst Synthesis
T. Keith Hollis; Li-Sheng Wang; Fook Tham; Journal of the American Chemical Society 122 (2000) 11737–11738; doi:10.1021/ja002411l

data_4116255
_publ_section_title
;
 Dynamic Resolution of a Metallocene: Diastereoselective Assembly of an
 Early-Late Heterobimetallic Metal-Bridgedansa-Metallocene Opening a Route
 to Parallel Catalyst Synthesis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11737
_journal_page_last               11738
_journal_paper_doi               10.1021/ja002411l
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C80 H80 Cl2 F6 O3 P4 Rh Sb Zr'
_chemical_formula_weight         1714.10
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.146(2)
_cell_angle_beta                 80.562(2)
_cell_angle_gamma                82.677(2)
_cell_formula_units_Z            2
_cell_length_a                   13.4053(11)
_cell_length_b                   16.3295(13)
_cell_length_c                   17.8203(14)
_cell_measurement_temperature    213(2)
_cell_volume                     3650.4(5)
_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      213(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0886
_diffrn_reflns_av_sigmaI/netI    0.0841
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45147
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.956
_exptl_absorpt_correction_T_max  0.9274
_exptl_absorpt_correction_T_min  0.7756
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_description       'Frag. of prism'
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          .08
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .28
_refine_diff_density_max         1.294
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.0168(7)
_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   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     888
_refine_ls_number_reflns         14354
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          2.040
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+0.7360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1584
_reflns_number_gt                9123
_reflns_number_total             14354
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja002411l.cif
_cod_data_source_block           kh21s
_cod_database_code               4116255