Olefin Polymerization Catalyst Derived by Activation of a Neutral Monoalkyl Titanium Complex with an Aminopyrrole Ligand Using Triisobutylaluminum and Trityl Borate
Yasumoto, Takahiro; Yamagata, Tsuneaki; Mashima, Kazushi; Chemistry Letters 36 (2007) 1030–; doi:10.1246/cl.2007.1030

data_8000138
_publ_section_title
;
 Olefin Polymerization Catalyst Derived by Activation of a Neutral
 Monoalkyl Titanium Complex with an Aminopyrrole Ligand Using
 Triisobutylaluminum and Trityl Borate
;
_journal_issue                   8
_journal_name_full               'Chemistry Letters'
_journal_page_first              1030
_journal_paper_doi               10.1246/cl.2007.1030
_journal_volume                  36
_journal_year                    2007
_chemical_formula_moiety         ' (C10 H15), (C13 H12 N2 O), Cl, Ti  '
_chemical_formula_structural     'Ti Cl (C5 (C H3)5) (C13 H12 N2 O) '
_chemical_formula_sum            'C22 H27 Cl N2 O Ti'
_chemical_formula_weight         418.81
_chemical_properties_physical    air-unstable
_chemical_temperature_decomposition_gt 330
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2004-02-16T14:42:47
_audit_creation_method           SHELXL-97
_audit_update_record             2006-09-16T15:56:00
_cell_angle_alpha                90.00
_cell_angle_beta                 92.31(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.351(4)
_cell_length_b                   22.339(14)
_cell_length_c                   24.788(12)
_cell_measurement_reflns_used    98182
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      3.00
_cell_volume                     4067(4)
_computing_cell_refinement       'Rigaku/RAPID Diffractometer Control'
_computing_data_collection       'Rigaku/RAPID Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_molecular_graphics    'Ortep-3 (Louis J. Farrugia, 1999)'
_computing_publication_material  'SHELXL-97 and modified'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1999)'
_computing_structure_solution
'SIR97(Altomare A., J. Appl. Cryst.,1999,32,115)'
_diffrn_ambient_temperature      120(1)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_details
;
RAPID: Eulerian 3-circle
;
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_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  0.1562
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            103276
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_T_max  0.9169
_exptl_absorpt_correction_T_min  0.8294
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Higashi, T. (1999). Shape - Program to obtain Crystal Shape using CCD
camera. Rigaku Corporation, Tokyo, Japan.
Higashi, T. (1999). Numabs - Numerical Absorption Correction, Rigaku
Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.060
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         9319
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1817
_refine_ls_R_factor_gt           0.1493
_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^)+(0.1170P)^2^+63.1484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3935
_refine_ls_wR_factor_ref         0.4082
_reflns_number_gt                6339
_reflns_number_total             9319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            36-1030sup1.cif
_cod_data_source_block           global
_cod_original_sg_symbol_H-M      'P21/n '
_cod_database_code               8000138