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_7027716
_publ_section_title
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 Synthesis and characterisation of titanium silasesquioxane complexes:
 soluble models for the active site in titanium silicate epoxidation
 catalysts&#x200A;&#x2020;
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_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            'C45 H86 O13 Si8 Ti'
_chemical_formula_weight         1107.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   16.955(4)
_cell_length_b                   16.955(4)
_cell_length_c                   17.853(6)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      14.0
_cell_measurement_theta_min      7.5
_cell_volume                     4445(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(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  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            1448
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         2.67
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.360
_exptl_absorpt_correction_T_max  .936
_exptl_absorpt_correction_T_min  .828
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_F_000             1782
_exptl_crystal_size_max          .42
_exptl_crystal_size_mid          .42
_exptl_crystal_size_min          .42
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.397
_refine_ls_goodness_of_fit_obs   1.655
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         1190
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.446
_refine_ls_restrained_S_obs      1.676
_refine_ls_R_factor_all          0.1535
_refine_ls_R_factor_obs          0.1071
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3075
_refine_ls_wR_factor_obs         0.2692
_reflns_number_observed          775
_reflns_number_total             1296
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            905887gsup1.cif
_cod_data_source_block           tresetti
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4444.6(21)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7027716