Dual-Excitation Polyoxometalate-Based Frameworks for One-Pot Light-Driven Hydrogen Evolution and Oxidative Dehydrogenation.
Sun, Wenlong; An, Bowen; Qi, Bo; Liu, Tao; Jin, Meng; Duan, Chunying; ACS applied materials & interfaces 10 (2018) 13462–13469; doi:10.1021/acsami.8b00350

data_4515355
_publ_section_title
;
 Dual-Excitation Polyoxometalate-Based Frameworks for One-Pot Light-Driven
 Hydrogen Evolution and Oxidative Dehydrogenation.
;
_journal_issue                   16
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              13462
_journal_page_last               13469
_journal_paper_doi               10.1021/acsami.8b00350
_journal_volume                  10
_journal_year                    2018
_chemical_formula_moiety         'C156 H108 N18 O92 P2 W18 Zn9'
_chemical_formula_sum            'C156 H108 N18 O92 P2 W18 Zn9'
_chemical_formula_weight         7666.17
_space_group_IT_number           175
_space_group_name_Hall           '-P 6'
_space_group_name_H-M_alt        'P 6/m'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P 6/m'
_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            1
_cell_length_a                   18.834(5)
_cell_length_b                   18.834(5)
_cell_length_c                   15.722(5)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.33
_cell_measurement_theta_min      2.50
_cell_volume                     4830(2)
_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-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30949
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.75
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    11.875
_exptl_absorpt_correction_T_max  0.241
_exptl_absorpt_correction_T_min  0.088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.636
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3538.0
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.867
_refine_diff_density_min         -2.504
_refine_diff_density_rms         0.313
_refine_ls_extinction_coef       0.00012(10)
_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   0.976
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3188
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1118P)^2^+291.3996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1866
_refine_ls_wR_factor_ref         0.2108
_reflns_number_gt                2722
_reflns_number_total             3188
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            am8b00350_si_003.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P6/m
_cod_database_code               4515355