Reduction-Induced Cyclization and Redox Reactions of Fully Methylated Titanocene Dichlorides Bearing Pendant Alkenyldimethylsilyl Groups, [TiCl2{η5-C5Me4(SiMe2R)}2] (R = Vinyl and Allyl)
Lukešová, Lenka; Štěpnička, Petr; Fejfarová, Karla; Gyepes, Róbert; Císařová, Ivana; Horáček, Michal; Kubišta, Jiří; Mach, Karel; Organometallics 21 (2002) 2639–; doi:10.1021/om020150d

data_4076858
_publ_section_title
;
 Reduction-Induced Cyclization and Redox Reactions of Fully Methylated
 Titanocene Dichlorides Bearing Pendant Alkenyldimethylsilyl Groups,
 [TiCl2{\h5-C5Me4(SiMe2R)}2] (R = Vinyl and Allyl)
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2639
_journal_paper_doi               10.1021/om020150d
_journal_volume                  21
_journal_year                    2002
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_sum            'C27 H45 O Si2 Ti'
_chemical_formula_weight         489.71
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.653(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.4010(11)
_cell_length_b                   15.4320(7)
_cell_length_c                   14.4340(5)
_cell_measurement_reflns_used    51888
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     5497.7(4)
_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(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26869
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.56
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.415
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         6225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+5.7681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1148
_reflns_number_gt                4727
_reflns_number_total             6225
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om020150d.cif
_cod_data_source_block           structure_12
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4076858