Bis(phenoxy-azo)titanium(IV) Complexes: Synthesis, Structure, and Catalytic Activity in Styrene Polymerization
Tanaka, Ryo; Viehmann, Philipp; Hecht, Stefan; Organometallics 31 (2012) 4216–; doi:10.1021/om3001636

data_4078431
_publ_section_title
;
 Bis(phenoxy-azo)titanium(IV) Complexes: Synthesis, Structure, and
 Catalytic Activity in Styrene Polymerization
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              4216
_journal_paper_doi               10.1021/om3001636
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C40 H50 Cl2 N4 O2 Ti'
_chemical_formula_sum            'C40 H50 Cl2 N4 O2 Ti'
_chemical_formula_weight         737.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           172
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 64'
_symmetry_space_group_name_H-M   'P 64'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   19.6254(4)
_cell_length_b                   19.6254(4)
_cell_length_c                   9.1641(2)
_cell_measurement_reflns_used    50101
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      3.27
_cell_volume                     3056.73(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      ' 231 frames, detector distance = 100 mm'
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1192
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            34685
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         3.27
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           45
_diffrn_source_power             2.25
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.378
_exptl_absorpt_correction_T_max  0.9104
_exptl_absorpt_correction_T_min  0.7952
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1170
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.387
_exptl_crystal_size_min          0.260
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         5151
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0569P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0832
_reflns_d_resolution_high        0.745
_reflns_d_resolution_low         6.231
_reflns_limit_h_max              13
_reflns_limit_h_min              -26
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              -12
_reflns_number_gt                4898
_reflns_number_total             5151
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3001636_si_001.cif
_cod_data_source_block           c:ta062-2
_cod_database_code               4078431