Chain Transfer to Solvent in Propene Polymerization with Ti Cp-phosphinimide Catalysts: Evidence for Chain Termination via Ti‒C Bond Homolysis
Ehm, Christian; Cipullo, Roberta; Passaro, Miriana; Zaccaria, Francesco; Budzelaar, Peter H. M.; Busico, Vincenzo; ACS Catalysis  (2016) 7989–; doi:10.1021/acscatal.6b02738

data_4513982
_publ_section_title
;
 Chain Transfer to Solvent in Propene Polymerization with Ti
 Cp-phosphinimide Catalysts: Evidence for Chain Termination via Ti--C Bond
 Homolysis
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              7989
_journal_paper_doi               10.1021/acscatal.6b02738
_journal_year                    2016
_chemical_formula_sum            'C34 H36 Cl2 N P Ti'
_chemical_formula_weight         608.41
_chemical_name_systematic
;
(pentamethylcyclopentadienyl)(triphenylphosphinimido)
titanium dichloride benzene solvate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   8.4630(19)
_cell_length_b                   20.965(8)
_cell_length_c                   35.984(12)
_cell_measurement_reflns_used    98
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.876
_cell_measurement_theta_min      3.493
_cell_volume                     6385(4)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al. 1999)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            29765
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.1
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  0.9415
_exptl_absorpt_correction_T_min  0.7851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Bruker 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         6855
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+4.9547P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.115
_reflns_number_gt                4614
_reflns_number_total             6855
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs6b02738_si_003.cif
_cod_data_source_block           phim
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4513982