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_4115558
_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            'C30 H28 Cl2 N2 Si Zr'
_chemical_formula_weight         606.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_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            8
_cell_length_a                   12.7198(2)
_cell_length_b                   12.7198(2)
_cell_length_c                   34.1068(2)
_cell_measurement_temperature    173(2)
_cell_volume                     5518.25(13)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            28557
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.658
_exptl_absorpt_correction_T_max  0.8797
_exptl_absorpt_correction_T_min  0.8271
_exptl_absorpt_correction_type   'empirical from SADABS'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       Block
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.006
_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          0.1280
_refine_ls_wR_factor_ref         0.1323
_reflns_number_gt                6328
_reflns_number_total             6582
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja004266h_1.cif
_cod_data_source_block           hmnt08
_cod_original_cell_volume        5518.25(6)
_cod_database_code               4115558