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_4110469
_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_sum            'C21 H39 Cl N2 Zr'
_chemical_formula_weight         446.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.584(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2180(13)
_cell_length_b                   16.162(2)
_cell_length_c                   15.474(2)
_cell_measurement_temperature    193(2)
_cell_volume                     2303.0(5)
_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      193(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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0116
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35921
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88064
_exptl_absorpt_correction_type   'empirical, SADABS'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_meas      0
_exptl_crystal_description       Block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.505
_exptl_crystal_size_mid          0.318
_exptl_crystal_size_min          0.304
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.0038(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         5271
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0208
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+0.8984P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0544
_reflns_number_gt                4989
_reflns_number_total             5271
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja057866vsi20051119_012213.cif
_cod_data_source_block           Cp*Zr(Cl)(iPr)[N(tBu)C(Me)N(Et)]
_cod_original_cell_volume        2302.9(5)
_cod_database_code               4110469