Formation of Trivalent Zirconocene Complexes fromansa-Zirconocene-Based Olefin-Polymerization Precatalysts: An EPR- and NMR-Spectroscopic Study
Taylor N. Lenton; John E. Bercaw; Valentina N. Panchenko; Vladimir A. Zakharov; Dmitrii E. Babushkin; Igor E. Soshnikov; Evgenii P. Talsi; Hans H. Brintzinger; Journal of the American Chemical Society 135 (2013) 10710–10719; doi:10.1021/ja403170u

data_4120139
_publ_section_title
;
 Formation of Trivalent Zirconocene Complexes fromansa-Zirconocene-Based
 Olefin-Polymerization Precatalysts: An EPR- and NMR-Spectroscopic Study
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10710
_journal_page_last               10719
_journal_paper_doi               10.1021/ja403170u
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C22 H24 Al Cl2 Si Zr'
_chemical_formula_weight         505.60
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 92.126(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9586(4)
_cell_length_b                   14.3029(6)
_cell_length_c                   14.1790(6)
_cell_measurement_reflns_used    8740
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.76
_cell_measurement_theta_min      2.34
_cell_volume                     2220.88(16)
_computing_cell_refinement       'SAINT V8.27B (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 2012.10-0 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT V8.27B (Bruker-AXS, 2007)'
_computing_molecular_graphics    'DIAMOND 3 (Crystal Impact, 1999)'
_computing_publication_material  'SHELXTL (Bruker-AXS, 2007)'
_computing_structure_refinement  'SHELXL-2012/8 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXT (Sheldrick, 2012)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0880
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            57055
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.108
_diffrn_reflns_theta_min         2.023
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2012/1 (Bruker-AXS, 2001)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       flake
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4888
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+3.9179P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3264
_reflns_number_total             4888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja403170u_si_002.cif
_cod_data_source_block           tnl17
_cod_database_code               4120139
_shelx_estimated_absorpt_t_min   0.823
_shelx_estimated_absorpt_t_max   0.936
_shelxl_version_number           2012-6
_shelx_res_checksum              1934