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_4073134
_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         'C35 H50 F20 Si5 Ti5'
_chemical_formula_sum            'C35 H50 F20 Si5 Ti5'
_chemical_formula_weight         1230.70
_chemical_melting_point          395
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 93.2874(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.07430(10)
_cell_length_b                   26.4287(2)
_cell_length_c                   26.6932(2)
_cell_measurement_reflns_used    22866
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     9912.61(13)
_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    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  '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  0.056
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            149981
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.45
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.994
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4960
_exptl_crystal_recrystallization_method 'crystallization from toluene/hexane'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1191
_refine_ls_number_reflns         22749
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+11.2888P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0929
_reflns_number_gt                16586
_reflns_number_total             22749
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om070098rsi20070226_082650.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4073134