Kinetic Resolution of Chiral α-Olefins Using Optically Active ansa-Zirconocene Polymerization Catalysts
Cliff R. Baar; Christopher J. Levy; Endy Y.-J. Min; Lawrence M. Henling; Michael W. Day; John E. Bercaw; Journal of the American Chemical Society 126 (2004) 8216–8231; doi:10.1021/ja040021j

data_4112712
_publ_section_title
;
 Kinetic Resolution of Chiral \a-Olefins Using Optically Active
 ansa-Zirconocene Polymerization Catalysts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8216
_journal_page_last               8231
_journal_paper_doi               10.1021/ja040021j
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C30 H50 Cl2 Si2 Zr, 0.5(C7 H8)'
_chemical_formula_sum            'C33.5 H54 Cl2 Si2 Zr'
_chemical_formula_weight         675.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_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                97.199(1)
_cell_angle_beta                 104.068(1)
_cell_angle_gamma                106.275(1)
_cell_formula_units_Z            2
_cell_length_a                   10.3602(5)
_cell_length_b                   13.1543(7)
_cell_length_c                   14.0843(7)
_cell_measurement_reflns_used    24577
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.19
_cell_volume                     1748.26(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART v5.054'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'Bruker SHELXTL v6.14'
_computing_structure_refinement  'Bruker SHELXTL v6.14'
_computing_structure_solution    'Bruker SHELXTL v5.1'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Bruker SMART 1000 ccd'
_diffrn_measurement_method       '\w scans at 7 fixed \f values'
_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  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39577
_diffrn_reflns_theta_full        28.18
_diffrn_reflns_theta_max         28.18
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        'within counting statistics'
_diffrn_standards_interval_time  'first scans recollected at end of runs'
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  0.9212
_exptl_absorpt_correction_T_min  0.8780
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       plate
_exptl_crystal_F_000             714
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.447
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     716
_refine_ls_number_reflns         15367
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.447
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/\s^2^(Fo^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0630
_reflns_number_gt                13420
_reflns_number_total             15367
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja040021j_c6.cif
_cod_data_source_block           (S)-6
_cod_original_formula_sum        'C33.50 H54 Cl2 Si2 Zr'
_cod_database_code               4112712