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_8000087
_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            'C27 H37 Cl2 O8 Si4 Ti2'
_chemical_formula_weight         768.63
_space_group_IT_number           2
_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                115.471(10)
_cell_angle_beta                 95.790(9)
_cell_angle_gamma                114.590(10)
_cell_formula_units_Z            2
_cell_length_a                   13.071(8)
_cell_length_b                   13.186(11)
_cell_length_c                   13.487(11)
_cell_measurement_temperature    293(2)
_cell_volume                     1794(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_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  0.0155
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14918
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.770
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             794
_refine_diff_density_max         0.685
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         7631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.093
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0903P)^2^+3.0480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1311
_reflns_number_gt                7417
_reflns_number_total             7631
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            34-1542sup1.cif
_cod_data_source_block           2
_cod_database_code               8000087