Self-Assembled Supramolecular Polyoxometalate Hybrid Architecture as a Multifunctional Oxidation Catalyst.
Ni, Lubin; Li, Huan; Xu, Hongjie; Shen, Chao; Liu, Ruzhang; Xie, Ju; Zhang, Fengmin; Chen, Chong; Zhao, Hongxia; Zuo, Tongfei; Diao, Guowang; ACS applied materials & interfaces 11 (2019) 38708–38718; doi:10.1021/acsami.9b12531

data_4514496
_publ_section_title
;
 Self-Assembled Supramolecular Polyoxometalate Hybrid Architecture as a
 Multifunctional Oxidation Catalyst.
;
_journal_issue                   42
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              38708
_journal_page_last               38718
_journal_paper_doi               10.1021/acsami.9b12531
_journal_volume                  11
_journal_year                    2019
_chemical_formula_sum            'C126 H210 Cl4 K Na7 O154 Si W12'
_chemical_formula_weight         6765.05
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_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-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.114(2)
_cell_length_b                   21.114
_cell_length_c                   44.213(5)
_cell_measurement_reflns_used    9546
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.4970
_cell_measurement_theta_min      2.2748
_cell_volume                     17070(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII area-detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            84290
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.566
_diffrn_reflns_theta_min         2.153
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.233
_exptl_absorpt_correction_T_max  0.393
_exptl_absorpt_correction_T_min  0.299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.974
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9792
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.510
_refine_diff_density_min         -1.488
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details
;
 Flack x determined using 7204 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.031(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     916
_refine_ls_number_reflns         17443
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+3.7462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0925
_reflns_Friedel_coverage         0.990
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                15704
_reflns_number_total             17443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am9b12531_si_002.cif
_cod_data_source_block           SiW12_CD
_cod_original_cell_volume        17069(4)
_cod_database_code               4514496
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              25737
_shelx_hkl_checksum              86035
_shelx_fab_checksum              72734