Synthesis and Structures of the First Titanium(IV) Complexes with Cyclic Tetrasiloxide Ligands: Incomplete and Complete Cage Titanosiloxanes
Hirotsu, Masakazu; Taruno, Shinsuke; Yoshimura, Takashi; Ueno, Keiji; Unno, Masafumi; Matsumoto, Hideyuki; Chemistry Letters 34 (2005) 1542–; doi:10.1246/cl.2005.1542

data_8000086
_publ_section_title
;
 Synthesis and Structures of the First Titanium(IV) Complexes with Cyclic
 Tetrasiloxide Ligands: Incomplete and Complete Cage Titanosiloxanes
;
_journal_issue                   11
_journal_name_full               'Chemistry Letters'
_journal_page_first              1542
_journal_paper_doi               10.1246/cl.2005.1542
_journal_volume                  34
_journal_year                    2005
_chemical_formula_sum            'C31 H39 O10.5 Si5 Ti'
_chemical_formula_weight         767.97
_space_group_IT_number           18
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4561(9)
_cell_length_b                   18.1710(9)
_cell_length_c                   14.1250(10)
_cell_measurement_temperature    293(2)
_cell_volume                     3710.4(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20382
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.445
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1604
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         10318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0755P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                9347
_reflns_number_total             10318
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            34-1542sup1.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C31 H39 O10.50 Si5 Ti'
_cod_database_code               8000086