Synthesis, Structure, and Olefin Polymerization Activity of Titanium Complexes Bearing Asymmetric Tetradentate [OSNO]-Type Bis(phenolato) Ligands
Geert-Jan M. Meppelder; Hong-Tao Fan; Thomas P. Spaniol; Jun Okuda; Inorganic Chemistry 48 (2009) 7378–7388; doi:10.1021/ic900903b

data_4302873
_publ_contact_author
;       Jun Okuda
        Institute of Inorganic Chemistry
        RWTH Aachen University
        Landoltweg 1
        D-52074 Aachen
        Germany
;
_publ_contact_author_email       jun.okuda@ac.rwth-aachen.de
_publ_contact_author_fax         '+49 241 80 92644'
_publ_contact_author_phone       '+49 241 80 94645'
_publ_section_title
;
Synthesis, Structure, and Olefin Polymerization Activity of Titanium
Complexes Bearing Asymmetric Tetradentate [OSNO]-Type Bis(phenolato) Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7378
_journal_page_last               7388
_journal_paper_doi               10.1021/ic900903b
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C35 H53 Cl2 N O2 S Ti, C2 H4 Cl4'
_chemical_formula_sum            'C37 H57 Cl6 N O2 S Ti'
_chemical_formula_weight         840.50
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4683(18)
_cell_length_b                   18.311(4)
_cell_length_c                   24.477(5)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      22.41
_cell_measurement_theta_min      2.37
_cell_volume                     4243.7(15)
_computing_cell_refinement       'Bruker SMART (2001)'
_computing_data_collection       'Bruker SMART (2001)'
_computing_data_reduction        'Bruker SAINT+ (1999)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR 97 (Altomare et al, 1997)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42001
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.660
_exptl_absorpt_correction_T_max  0.9250
_exptl_absorpt_correction_T_min  0.7423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.497
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       0.0048(7)
_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   1.157
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         5305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0882
_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^)+(0.0867P)^2^+13.5065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2215
_refine_ls_wR_factor_ref         0.2349
_reflns_number_gt                4461
_reflns_number_total             5305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900903b_si_002_2.cif
_cod_data_source_block           7b
_cod_database_code               4302873