Bis(imidodithiodiphosphinato) Titanium and Zirconium Complexes: Synthesis, Characterization, and Their Catalytic Activity in the Polymerization of α-Olefins
Chen, Fapu; Kapon, Moshe; Woollins, J. Derek; Eisen, Moris S.; Organometallics 28 (2009) 2391–; doi:10.1021/om801176a

data_4068953
_publ_section_title
;
 Bis(imidodithiodiphosphinato) Titanium and Zirconium Complexes:
 Synthesis, Characterization, and Their Catalytic Activity in the
 Polymerization of \a-Olefins
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2391
_journal_paper_doi               10.1021/om801176a
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C50 H45 N3 P4 S4 Ti'
_chemical_formula_sum            'C50 H45 N3 P4 S4 Ti'
_chemical_formula_weight         987.91
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.620(10)
_cell_angle_beta                 68.630(8)
_cell_angle_gamma                82.190(7)
_cell_formula_units_Z            2
_cell_length_a                   11.906(2)
_cell_length_b                   13.980(2)
_cell_length_c                   16.088(2)
_cell_measurement_reflns_used    23008
_cell_measurement_temperature    230.0(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_volume                     2438.6(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Nonius (1997), KappaCCD Collect Program'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_molecular_graphics
;
Molecular Structure Corporation (1999). 
ORTEP. TEXRAY Structure Analysis Package. 
MSC, 3200 Research Forest Drive, The 
Woodlands,TX 77381, USA.
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
S.Mackay, C.J.Gilmore, C.Edwards, M. Tremayne, N. Stuart, K.Shankland 
"maXus": a computer program for the solution and refinement of crystal 
structures from diffraction data University of Glasgow, Scotland, UK, 
Nonius BV, Delft, The Netherlands and MacScience Co. Ltd.,
Yokohama, Japan (1998)
;
_diffrn_ambient_temperature      230.0(1)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2592
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8562
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_T_max  0.9502
_exptl_absorpt_correction_T_min  0.9266
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.0011(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   0.872
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         8562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.872
_refine_ls_R_factor_all          0.2193
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0828P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.2054
_reflns_number_gt                2882
_reflns_number_total             8562
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801176a_si_004.cif
_cod_data_source_block           tidips
_cod_database_code               4068953