Synthesis of Half-Titanocenes Containing 1,3-Imidazolidin-2-Iminato Ligands of type, Cp*TiCl2[1,3-R2(CH2N)2C=N]: Highly Active Catalyst Precursors in Ethylene (Co)polymerisation
Nomura, Kotohiro; Patamma, Srisuda; Matsuda, Hideshi; Katao, Shohei; Tsutsumi, Ken; Fukuda, Hiroya; RSC Adv.  (2015) –; doi:10.1039/C5RA11402K

data_7221619
_publ_section_title
;
 Synthesis of Half-Titanocenes Containing 1,3-Imidazolidin-2-Iminato
 Ligands of type, Cp*TiCl2[1,3-R2(CH2N)2C=N]: Highly Active Catalyst
 Precursors in Ethylene (Co)polymerisation
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA11402K
_journal_year                    2015
_chemical_formula_moiety         'C37 H53 Cl2 N3 Ti, 2(C Cl2)'
_chemical_formula_sum            'C39 H53 Cl6 N3 Ti'
_chemical_formula_weight         824.49
_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_update_record
;
2015-05-26 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                94.0438(7)
_cell_angle_beta                 100.1681(7)
_cell_angle_gamma                115.2973(7)
_cell_formula_units_Z            2
_cell_length_a                   11.1642(2)
_cell_length_b                   11.2931(2)
_cell_length_c                   19.4433(4)
_cell_measurement_reflns_used    32699
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.15
_cell_volume                     2151.95(7)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37405
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.823
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             864.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.080
_refine_diff_density_min         -0.490
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     511
_refine_ls_number_reflns         9868
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0683P)^2^+0.9296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1224
_reflns_number_gt                8961
_reflns_number_total             9868
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c5ra11402k2.cif
_cod_data_source_block           CpsiPr2Ph2NTiCl2
_cod_original_cell_volume        2151.93(7)
_cod_database_code               7221619