New Titanium and Hafnium Complexes Bearing [−NNN–] Pyrrolylpyridylamido Ligands as Olefin Polymerization Catalysts
Li, Gang; Lamberti, Marina; Roviello, Giuseppina; Pellecchia, Claudio; Organometallics 31 (2012) 6772–; doi:10.1021/om300519s

data_4079144
_publ_section_title
;
 New Titanium and Hafnium Complexes Bearing [&#x2212;NNN--]
 Pyrrolylpyridylamido Ligands as Olefin Polymerization Catalysts
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              6772
_journal_paper_doi               10.1021/om300519s
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C35 H47 Hf N5'
_chemical_formula_sum            'C35 H47 Hf N5'
_chemical_formula_weight         716.27
_chemical_name_systematic
;
(2,6-diisopropyl-phenyl)-[(2-isopropyl-phenyl)-[6-(1H-pyrrol-2-yl)-
pyridin-2-yl]-methyl]-amine-bis(dimethylamino)
-Hafnium
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   35.772(2)
_cell_length_b                   13.073(3)
_cell_length_c                   14.102(5)
_cell_measurement_reflns_used    406
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.045
_cell_measurement_theta_min      3.459
_cell_volume                     6595(3)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34264
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.11
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.194
_exptl_absorpt_correction_T_max  0.4475
_exptl_absorpt_correction_T_min  0.2981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (Bruker, 2000)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         13707
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0087P)^2^+5.7338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0501
_refine_ls_wR_factor_ref         0.0516
_reflns_number_gt                12371
_reflns_number_total             13707
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om300519s_si_002.cif
_cod_data_source_block           ganghf
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               4079144