Living Ziegler-Natta Polymerization by Early Transition Metals: Synthesis and Evaluation of Cationic Zirconium Alkyl Complexes Bearing β-Hydrogens as Models for Propagating Centers
Matthew B. Harney; Richard J. Keaton; James C. Fettinger; Lawrence R. Sita; Journal of the American Chemical Society 128 (2006) 3420–3432; doi:10.1021/ja057866v

data_4110477
_publ_section_title
;
 Living Ziegler-Natta Polymerization by Early Transition Metals: Synthesis
 and Evaluation of Cationic Zirconium Alkyl Complexes Bearing \b-Hydrogens
 as Models for Propagating Centers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3420
_journal_page_last               3432
_journal_paper_doi               10.1021/ja057866v
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C46 H41 B F20 N2 Zr'
_chemical_formula_sum            'C46 H41 B F20 N2 Zr'
_chemical_formula_weight         1103.84
_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                70.9290(10)
_cell_angle_beta                 72.1160(10)
_cell_angle_gamma                77.0170(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2046(8)
_cell_length_b                   13.3258(9)
_cell_length_c                   17.3270(12)
_cell_measurement_reflns_used    8476
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.428
_cell_measurement_theta_min      2.349
_cell_volume                     2304.6(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 0.999
_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         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21038
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  0.9539
_exptl_absorpt_correction_T_min  0.9110
_exptl_absorpt_correction_type   'empirical, SADABS (multi-scan)'
_exptl_absorpt_process_details   'Blessing,R.H.(1995).Acta Cryst.,A51,33-38.'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_meas      0
_exptl_crystal_description       Block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.164
_refine_diff_density_min         -0.956
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         10584
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0904P)^2^+0.1078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1323
_reflns_number_gt                8573
_reflns_number_total             10584
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja057866vsi20051119_012353.cif
_cod_data_source_block           {Cp*Zr(iBu)[N(tBu)C(Me)N(Et)]}[B(C6F5)4]
_cod_database_code               4110477