Reactivity Studies, Structural Characterization, and Thermolysis of Cubic Titanosiloxanes: Precursors to Titanosilicate Materials Which Catalyze Olefin Epoxidation
Ramaswamy Murugavel; Paul Davis; Vivekanand S. Shete; Inorganic Chemistry 42 (2003) 4696–4706; doi:10.1021/ic034317m

data_4313920
_publ_section_title
;
 Reactivity Studies, Structural Characterization, and Thermolysis of Cubic
 Titanosiloxanes: Precursors to Titanosilicate Materials Which Catalyze
 Olefin Epoxidation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4696
_journal_page_last               4706
_journal_paper_doi               10.1021/ic034317m
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C72 H132 N4 O16 Si8 Ti4'
_chemical_formula_weight         1726.14
_space_group_IT_number           220
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I -4bd 2c 3'
_symmetry_space_group_name_H-M   'I -4 3 d'
_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            12
_cell_length_a                   31.702
_cell_length_b                   31.702
_cell_length_c                   31.702
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.56
_cell_measurement_theta_min      8.29
_cell_volume                     31861.043
_computing_cell_refinement       'Enraf Nonius CAD4, 1989'
_computing_data_collection       'Enraf Nonius CAD4, 1989'
_computing_data_reduction        'maXus (Mackay et al., 1999)'
_computing_molecular_graphics    'maXus (Mackay et al., 1999)'
_computing_publication_material  'maXus (Mackay et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CAD4 MACH3'
_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  0.0698
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14237
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.430
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             11040
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(7)
_refine_ls_extinction_coef       0.00014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         2482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0936P)^2^+22.0507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1622
_reflns_number_gt                1732
_reflns_number_total             2482
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034317msi20030325_120849_1.cif
_cod_data_source_block           rm005a(Compound1)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        31860.7
_cod_database_code               4313920