Evaluation of the Oxygen π-Donation in Permethyltitanocene Silanolates and Alcoholates
Varga, Vojtech; Císařová, Ivana; Gyepes, Róbert; Horáček, Michal; Kubišta, Jiří; Mach, Karel; Organometallics 28 (2009) 1748–; doi:10.1021/om801209f

data_4069031
_publ_section_title
;
 Evaluation of the Oxygen \p-Donation in Permethyltitanocene Silanolates
 and Alcoholates
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1748
_journal_paper_doi               10.1021/om801209f
_journal_volume                  28
_journal_year                    2009
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'C32 H57 O4 Si Ti'
_chemical_formula_sum            'C32 H57 O4 Si Ti'
_chemical_formula_weight         581.77
_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                83.5103(11)
_cell_angle_beta                 87.7159(11)
_cell_angle_gamma                69.6085(10)
_cell_formula_units_Z            2
_cell_length_a                   10.5233(2)
_cell_length_b                   11.1081(2)
_cell_length_c                   15.3903(3)
_cell_measurement_reflns_used    7540
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1675.49(6)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.037
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36181
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.33
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.323
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green-braun
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             634
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         7713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0416P)^2^+0.7777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0901
_reflns_number_gt                6751
_reflns_number_total             7713
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om801209f_si_001.cif
_cod_data_source_block           jednositbu-mach_structure_4
_cod_original_cell_volume        1675.49(5)
_cod_database_code               4069031