Chiral Ansa Metallocenes with Cp Ring-Fused to Thiophenes and Pyrroles: Syntheses, Crystal Structures, and Isotactic Polypropylene Catalysts
John A. Ewen; Michael J. Elder; Robert L. Jones; Arnold L. Rheingold; Louise M. Liable-Sands; Roger D. Sommer; Journal of the American Chemical Society 123 (2001) 4763–4773; doi:10.1021/ja004266h

data_4115559
_publ_section_title
;
 Chiral Ansa Metallocenes with Cp Ring-Fused to Thiophenes and Pyrroles:
 Syntheses, Crystal Structures, and Isotactic Polypropylene Catalysts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4763
_journal_page_last               4773
_journal_paper_doi               10.1021/ja004266h
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C32 H30 Cl2 S2 Si Zr'
_chemical_formula_weight         668.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 91.6932(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5183(2)
_cell_length_b                   35.7383(3)
_cell_length_c                   8.8314(2)
_cell_measurement_temperature    243(2)
_cell_volume                     3002.85(10)
_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      243(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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  0.0690
_diffrn_reflns_av_sigmaI/netI    0.0723
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10660
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_T_max  0.9780
_exptl_absorpt_correction_T_min  0.8654
_exptl_absorpt_correction_type   'empirical from SADABS'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.808
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.808
_refine_ls_R_factor_all          0.1318
_refine_ls_R_factor_gt           0.0985
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2486
_refine_ls_wR_factor_ref         0.2727
_reflns_number_gt                3559
_reflns_number_total             4560
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja004266h_2.cif
_cod_data_source_block           hmnt10r
_cod_original_cell_volume        3002.85(7)
_cod_database_code               4115559