Synthesis and characterisation of titanium silasesquioxane complexes: soluble models for the active site in titanium silicate epoxidation catalysts †
Crocker, Mark; Herold, Ruud H. M.; Orpen, A. Guy; Overgaag, Martijn T. A.; Journal of the Chemical Society, Dalton Transactions  (1999) 3791–; doi:10.1039/a905887g

data_7027717
_publ_section_title
;
 Synthesis and characterisation of titanium silasesquioxane complexes:
 soluble models for the active site in titanium silicate epoxidation
 catalysts&#x200A;&#x2020;
;
_journal_issue                   21
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3791
_journal_paper_doi               10.1039/a905887g
_journal_year                    1999
_chemical_formula_sum            'C97 H180 O24 Si16 Ti'
_chemical_formula_weight         2227.75
_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
_cell_angle_alpha                73.86(3)
_cell_angle_beta                 77.13(3)
_cell_angle_gamma                87.37(3)
_cell_formula_units_Z            4
_cell_length_a                   21.085(8)
_cell_length_b                   22.498(8)
_cell_length_c                   27.786(10)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      8.0
_cell_volume                     12341(8)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       R3m
_diffrn_measurement_method       'Wyckoff w scan'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0751
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            32278
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_F_000             4800
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.215
_refine_diff_density_min         -1.409
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.414
_refine_ls_goodness_of_fit_obs   1.695
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     2378
_refine_ls_number_reflns         32260
_refine_ls_number_restraints     1559
_refine_ls_restrained_S_all      1.412
_refine_ls_restrained_S_obs      1.665
_refine_ls_R_factor_all          0.2097
_refine_ls_R_factor_obs          0.1342
_refine_ls_shift/esd_max         0.401
_refine_ls_shift/esd_mean        0.041
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; calc 
 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+100.0000+100.0000*P+(0.0700P)^2^+0.0000sin\q/\l] 
 where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_wR_factor_all         0.3476
_refine_ls_wR_factor_obs         0.3042
_reflns_number_observed          18023
_reflns_number_total             32278
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            905887gsup1.cif
_cod_data_source_block           trentunot
_cod_original_cell_volume        12341.5(78)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7027717