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_7221618
_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         '4(C29 H37 Cl2 N3 Ti), C Cl2'
_chemical_formula_sum            'C117 H148 Cl10 N12 Ti4'
_chemical_formula_weight         2268.67
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      18
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   21.8842(5)
_cell_length_b                   28.7235(7)
_cell_length_c                   9.4156(2)
_cell_measurement_reflns_used    45903
_cell_measurement_temperature    213
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.04
_cell_volume                     5918.6(2)
_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    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      213
_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  0.0309
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            58490
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2384.00
_exptl_crystal_size_max          0.620
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.640
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  6051 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.024(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     643
_refine_ls_number_reflns         13519
_refine_ls_number_restraints     3
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0537P)^2^+1.5844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0971
_reflns_number_gt                12432
_reflns_number_total             13519
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c5ra11402k2.cif
_cod_data_source_block           CpS-36(26-Me2Ph)2NHC
_cod_original_cell_volume        5918.6(3)
_cod_database_code               7221618