Fluorosilyl-Substituted Cyclopentadienyltitanium(IV) Complexes: Synthesis, Structure, and Styrene Polymerization Behavior#
Erben, Milan; Merna, Jan; Hermanová, Soňa; Císařová, Ivana; Padělková, Zdeňka; Dušek, Michal; Organometallics 26 (2007) 2735–; doi:10.1021/om070098r

data_4073133
_publ_section_title
;
 Fluorosilyl-Substituted Cyclopentadienyltitanium(IV) Complexes:&#x00A0;
 Synthesis, Structure, and Styrene Polymerization Behavior#
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2735
_journal_paper_doi               10.1021/om070098r
_journal_volume                  26
_journal_year                    2007
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C7 H10 Cl3 F Si Ti'
_chemical_formula_sum            'C7 H10 Cl3 F Si Ti'
_chemical_formula_weight         295.49
_chemical_melting_point          344
_chemical_name_systematic
trichloro-(h5-dimethylfluorosilylcyclopentadienyl)titanum(IV)
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                96.361(5)
_cell_angle_beta                 92.040(5)
_cell_angle_gamma                104.006(4)
_cell_formula_units_Z            4
_cell_length_a                   6.4370(3)
_cell_length_b                   12.5910(5)
_cell_length_c                   14.9830(10)
_cell_measurement_reflns_used    17673
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1168.54(11)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17674
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.37
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.486
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sortav
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_recrystallization_method
'sublimation in ampoule at 1 Pa / 315 K'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         5358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.228
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0499P)^2^+0.1853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.1125
_reflns_number_gt                4051
_reflns_number_total             5358
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om070098rsi20070226_082650.cif
_cod_data_source_block           I
_cod_database_code               4073133