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_4076859
_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            'C26 H42 Cl2 Si2 Ti'
_chemical_formula_weight         529.58
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.5240(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.1660(2)
_cell_length_b                   32.0790(7)
_cell_length_c                   10.7310(2)
_cell_measurement_reflns_used    105746
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1
_cell_volume                     2733.12(10)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0696
_diffrn_reflns_av_sigmaI/netI    0.0595
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            25642
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.05
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0362P)^2^+3.4465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1159
_reflns_number_gt                3828
_reflns_number_total             4810
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om020150d.cif
_cod_data_source_block           structure_14
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4076859