Intra- and Intermolecular NMR Studies on the Activation of Arylcyclometallated Hafnium Pyridyl-Amido Olefin Polymerization Precatalysts
Cristiano Zuccaccia; Alceo Macchioni; Vincenzo Busico; Roberta Cipullo; Giovanni Talarico; Francesca Alfano; Harold W. Boone; Kevin A. Frazier; Phillip D. Hustad; James C. Stevens; Paul C. Vosejpka; Khalil A. Abboud; Journal of the American Chemical Society 130 (2008) 10354–10368; doi:10.1021/ja802072n

data_4108133
_publ_section_title
;
 Intra- and Intermolecular NMR Studies on the Activation of
 Arylcyclometallated Hafnium Pyridyl-Amido Olefin Polymerization
 Precatalysts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10354
_journal_page_last               10368
_journal_paper_doi               10.1021/ja802072n
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C77 H61 B F20 Hf N2'
_chemical_formula_weight         1583.58
_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                73.652(1)
_cell_angle_beta                 79.656(1)
_cell_angle_gamma                62.921(1)
_cell_formula_units_Z            2
_cell_length_a                   14.4141(7)
_cell_length_b                   15.6207(8)
_cell_length_c                   17.4973(9)
_cell_measurement_reflns_used    306
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     3359.9(3)
_computing_cell_refinement
'Bruker SMART v5.624 & SAINT 6.36a (Bruker 1998)'
_computing_data_collection       'Bruker SMART v5.624 (Bruker 1998)'
_computing_data_reduction        'Bruker SHELXTL v6.14 (Bruker 2000)'
_computing_molecular_graphics    'Bruker SHELXTL v6.14'
_computing_publication_material  'Bruker SHELXTL v6.14'
_computing_structure_refinement  'Bruker SHELXTL v6.14'
_computing_structure_solution    'Bruker SHELXTL v6.14'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'SMART CCD area detector'
_diffrn_measurement_method       '\w 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  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22028
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        1
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.655
_exptl_absorpt_correction_T_max  0.8868
_exptl_absorpt_correction_T_min  0.7459
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL  v6.12 (Bruker 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_meas      0
_exptl_crystal_description       plates
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         15030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0639
_reflns_number_gt                13243
_reflns_number_total             15030
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja802072n-file001.cif
_cod_data_source_block           macc7
_cod_database_code               4108133