Unveiling the Active Surface Sites in Heterogeneous Titanium-Based Silicalite Epoxidation Catalysts: Input of Silanol-Functionalized Polyoxotungstates as Soluble Analogues
Zhang, Teng; Mazaud, Louis; Chamoreau, Lise-Marie; Paris, Céline; Proust, Anna; Guillemot, Geoffroy; ACS Catalysis 8 (2018) 2330–; doi:10.1021/acscatal.8b00256

data_4514398
_publ_section_title
;
 Unveiling the Active Surface Sites in Heterogeneous Titanium-Based
 Silicalite Epoxidation Catalysts: Input of Silanol-Functionalized
 Polyoxotungstates as Soluble Analogues
;
_journal_issue                   3
_journal_name_full               'ACS Catalysis'
_journal_page_first              2330
_journal_paper_doi               10.1021/acscatal.8b00256
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C15 H34 O38 P Si3 Ti W9,3 (C24 H52 N)'
_chemical_formula_sum            'C87 H190 N3 O38 P Si3 Ti W9'
_chemical_formula_weight         3704.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.2301(17)
_cell_length_b                   28.431(2)
_cell_length_c                   43.025(3)
_cell_measurement_reflns_used    9811
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      33.22
_cell_measurement_theta_min      3.19
_cell_volume                     24746(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            432631
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.288
_diffrn_reflns_theta_min         2.137
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    8.503
_exptl_absorpt_correction_T_max  0.16
_exptl_absorpt_correction_T_min  0.08
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS, Bruker AXS Inc., Madison, 
Wisconsin, USA. 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.988
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             14256
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.807
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1331
_refine_ls_number_reflns         47463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0077P)^2^+61.2127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0460
_refine_ls_wR_factor_ref         0.0506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                37485
_reflns_number_total             47463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b00256_si_002.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 4514398.cif.'
_cod_database_code               4514398
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              81807
_shelx_hkl_checksum              13217