Synthesis of Hafnium and Zirconium Imino−Amido Complexes from Bis-imine Ligands. A New Family of Olefin Polymerization Catalysts
De Waele, Philip; Jazdzewski, Brian A.; Klosin, Jerzy; Murray, Rex E.; Theriault, Curt N.; Vosejpka, Paul C.; Petersen, Jeffrey L.; Organometallics 26 (2007) 3896–; doi:10.1021/om7004723

data_4073572
_publ_section_title
;
 Synthesis of Hafnium and Zirconium Imino&#x2212;Amido Complexes from
 Bis-imine Ligands. A New Family of Olefin Polymerization Catalysts
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3896
_journal_paper_doi               10.1021/om7004723
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C54 H64 N2 Zr'
_chemical_formula_weight         832.29
_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                 91.016(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5237(10)
_cell_length_b                   18.2574(14)
_cell_length_c                   18.3733(14)
_cell_measurement_reflns_used    6962
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.50
_cell_volume                     4535.8(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0632
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30152
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.280
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         10186
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0464P)^2^+1.7024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1170
_reflns_number_gt                8458
_reflns_number_total             10186
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7004723-file002.cif
_cod_data_source_block           13
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4073572