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_7221617
_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         'C25 H29 Cl2 N3 Ti'
_chemical_formula_sum            'C25 H29 Cl2 N3 Ti'
_chemical_formula_weight         490.33
_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_update_record
;
2015-05-26 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 94.0965(9)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.6563(3)
_cell_length_b                   7.42574(18)
_cell_length_c                   36.5572(10)
_cell_measurement_reflns_used    20249
_cell_measurement_temperature    123
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.21
_cell_volume                     2343.87(12)
_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    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0264
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            22274
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1024.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.310
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5362
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0476P)^2^+0.8443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0968
_reflns_number_gt                4574
_reflns_number_total             5362
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c5ra11402k2.cif
_cod_data_source_block           Cps-36Ph2NHC
_cod_original_cell_volume        2343.86(11)
_cod_database_code               7221617