Synthesis and oxidation catalysis of a Ti-substituted phosphotungstate, and identification of the active oxygen species
Takahashi, Eri; Kamata, Keigo; Kikukawa, Yuji; Sato, Sota; Suzuki, Kosuke; Yamaguchi, Kazuya; Mizuno, Noritaka; Catal. Sci. Technol. 5 (2015) 4778–; doi:10.1039/C5CY01031D

data_1529376
_publ_section_title
;
 Synthesis and oxidation catalysis of a Ti-substituted phosphotungstate,
 and identification of the active oxygen species
;
_journal_issue                   10
_journal_name_full               'Catal. Sci. Technol.'
_journal_page_first              4778
_journal_paper_doi               10.1039/C5CY01031D
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety         'O80 P2 Ti4 W20'
_chemical_formula_sum            'O80 P2 Ti4 W20'
_chemical_formula_weight         5210.54
_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   none
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-06-11 deposited with the CCDC.
2015-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                88.88(3)
_cell_angle_beta                 85.12(3)
_cell_angle_gamma                79.80(3)
_cell_formula_units_Z            8
_cell_length_a                   20.570(4)
_cell_length_b                   34.716(7)
_cell_length_c                   54.711(11)
_cell_measurement_reflns_used    32795
_cell_measurement_temperature    95(2)
_cell_volume                     38312(14)
_computing_cell_refinement       HKL2000
_computing_data_collection       'KEK uguis'
_computing_data_reduction        HKL2000
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      95(2)
_diffrn_measured_fraction_theta_full 0.847
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_details
;
'1.00 degrees, 0.1 sec, detector distance 111.20 mm'
;
_diffrn_measurement_device_type  'PAD Pilatus 2M-F (Dectris)'
_diffrn_measurement_method       'oscillation method, w scans'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_source         'KEK PF BL1A beamline'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.95000
_diffrn_reflns_av_R_equivalents  0.1028
_diffrn_reflns_av_sigmaI/netI    0.1847
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            84195
_diffrn_reflns_theta_full        25.64
_diffrn_reflns_theta_max         25.64
_diffrn_reflns_theta_min         0.80
_exptl_absorpt_coefficient_mu    25.366
_exptl_absorpt_correction_T_max  0.1858
_exptl_absorpt_correction_T_min  0.0806
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL2000 DENZO SCALEPACK'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             17904
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         1.666
_refine_diff_density_min         -1.973
_refine_diff_density_rms         0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3817
_refine_ls_number_reflns         51400
_refine_ls_number_restraints     3741
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.1414
_refine_ls_R_factor_gt           0.0999
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1023P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2311
_refine_ls_wR_factor_ref         0.2470
_reflns_number_gt                25506
_reflns_number_total             51400
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cy01031d2.cif
_cod_data_source_block           II
_cod_depositor_comments
'Adding full bibliography for 1529375--1529376.cif.'
_cod_original_cell_volume        38312(13)
_cod_database_code               1529376