Benzylation of α-Diimine Ligands Bound to Zirconium and Hafnium. A New Convenient Route to Olefin Polymerization Catalysts
Mashima, Kazushi; Ohnishi, Ryuji; Yamagata, Tsuneaki; Tsurugi, Hayato; Chemistry Letters 36 (2007) 1420–; doi:10.1246/cl.2007.1420

data_8000154
_publ_section_title
;
 Benzylation of \a-Diimine Ligands Bound to Zirconium and Hafnium. A New
 Convenient Route to Olefin Polymerization Catalysts
;
_journal_issue                   12
_journal_name_full               'Chemistry Letters'
_journal_page_first              1420
_journal_paper_doi               10.1246/cl.2007.1420
_journal_volume                  36
_journal_year                    2007
_chemical_formula_moiety         ' (C7 H7)3, (C25 H27 N2), Zr1, (C7 H8) '
_chemical_formula_structural     '(Zr1 3(C7 H7) (C25 H27 N2)) (C7 H8)'
_chemical_formula_sum            'C53 H56 N2 Zr'
_chemical_formula_weight         812.22
_chemical_properties_physical    air-unstable
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2006-09-06T14:15:29
_audit_creation_method
'from SHELXL97 CIF and IUCr SHELXL97-template'
_audit_update_record
;
2006-09-20 16:17

2006-09-21T15:27 # Formatted by publCIF
;
_cell_angle_alpha                97.217(2)
_cell_angle_beta                 97.205(2)
_cell_angle_gamma                108.524(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0235(7)
_cell_length_b                   12.4819(8)
_cell_length_c                   16.7108(12)
_cell_measurement_reflns_used    25568
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      30.45
_cell_measurement_theta_min      3.05
_cell_volume                     2129.2(2)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.1200
_diffrn_reflns_av_sigmaI/netI    0.0915
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            58031
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        30.48
_diffrn_reflns_theta_max         30.48
_diffrn_reflns_theta_min         3.04
_diffrn_source_current           40
_diffrn_source_power             50
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.785
_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    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             856
_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 toluene at 255 K under Ar'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.041
_refine_diff_density_min         -1.200
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       0.0073(10)
_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   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         12915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0681
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+2.9938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1714
_reflns_number_gt                8869
_reflns_number_total             12915
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            36-1420sup1.cif
_cod_data_source_block           global
_cod_original_sg_symbol_Hall     '  -P 1 '
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8000154