Large Polyoxotitanate Clusters: Well-Defined Models for Pure-Phase TiO2Structures and Surfaces
Jason B. Benedict; Renata Freindorf; Elzbieta Trzop; Jeffrey Cogswell; Philip Coppens; Journal of the American Chemical Society 132 (2010) 13669–13671; doi:10.1021/ja106436y

data_4103182
_publ_section_title
;
 Large Polyoxotitanate Clusters: Well-Defined Models for Pure-Phase
 TiO2Structures and Surfaces
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13669
_journal_page_last               13671
_journal_paper_doi               10.1021/ja106436y
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C104 H216 O84 Ti28, C7 H8'
_chemical_formula_sum            'C111 H224 O84 Ti28'
_chemical_formula_weight         4244.10
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   29.7286(8)
_cell_length_b                   29.7286(8)
_cell_length_c                   126.826(3)
_cell_measurement_reflns_used    9050
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.19
_cell_volume                     97071(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       154
_diffrn_reflns_limit_l_min       -154
_diffrn_reflns_number            359456
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.71
_diffrn_reflns_theta_min         0.96
_exptl_absorpt_coefficient_mu    1.043
_exptl_absorpt_correction_T_max  0.9029
_exptl_absorpt_correction_T_min  0.8186
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             39204
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.776
_refine_diff_density_min         -1.175
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1027
_refine_ls_number_reflns         20567
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1037P)^2^+1145.8513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.1989
_reflns_number_gt                16935
_reflns_number_total             20567
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja106436y_si_001_3.cif
_cod_data_source_block           Ti28
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4103182