Controlled Benzylation of α-Diimine Ligands Bound to Zirconium and Hafnium: An Alternative Method for Preparing Mono- and Bis(amido)M(CH2Ph)n(n= 2, 3) Complexes as Catalyst Precursors for Isospecific Polymerization of α-Olefins
Tsurugi, Hayato; Ohnishi, Ryuji; Kaneko, Hiroshi; Panda, Tarun K.; Mashima, Kazushi; Organometallics 28 (2009) 680–; doi:10.1021/om800880n

data_4068476
_publ_section_title
;
 Controlled Benzylation of \a-Diimine Ligands Bound to Zirconium and
 Hafnium: An Alternative Method for Preparing Mono- and
 Bis(amido)M(CH2Ph)n(n= 2, 3) Complexes as Catalyst Precursors for
 Isospecific Polymerization of \a-Olefins
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              680
_journal_paper_doi               10.1021/om800880n
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C58 H72 N2 Zr'
_chemical_formula_weight         888.40
_chemical_properties_physical    air-unstable
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_date             2006-09-09T08:49:18
_audit_creation_method
'from SHELXL97 CIF and IUCr SHELXL97-template'
_audit_update_record
;
2006-09-12T15:02

2006-09-15T14:45 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.429(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7079(8)
_cell_length_b                   17.9374(12)
_cell_length_c                   22.2068(14)
_cell_measurement_reflns_used    48841
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      30.45
_cell_measurement_theta_min      3.0
_cell_volume                     5019.5(6)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        ' teXan (Rigaku/MSC, 2004) '
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  ' SHELXL-97 (Sheldrick, 1997) and modified '
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    ' SIR2004 (Maria et al., 2005) '
_diffrn_ambient_temperature      120(1)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_details
;
RAPID: Eulerian 3-circle
;
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_collimation    ' 0.8 mm double pinhole '
_diffrn_radiation_detector       'imaging plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.2282
_diffrn_reflns_av_sigmaI/netI    0.2137
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            143982
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.00
_diffrn_source_current           40
_diffrn_source_power             50
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
Higashi, H. (1995), ABSCOR: Program for Absorption 
Correction, Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       ' platelet '
_exptl_crystal_F_000             1896
_exptl_crystal_preparation
'mounted on the CryoLoop with mineral oil and placed in N2 stream at 120(1) K'
_exptl_crystal_recrystallization_method
'Crystallized from a solution of hexane at ambient temperature under Ar'
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.786
_refine_diff_density_min         -1.515
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.0111(8)
_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   0.871
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         15226
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.871
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1453
_reflns_number_gt                7568
_reflns_number_total             15226
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800880n_si_001.cif
_cod_data_source_block           global
_cod_original_sg_symbol_Hall     ' -P 2yn '
_cod_original_sg_symbol_H-M      ' P21/n '
_cod_database_code               4068476