Synthesis and photo-/electro-catalytic properties of Keggin polyoxometalate inorganic-organic hybrid layers based on d10 metal and rigid benzo-diazole/-triazole ligands
Cao, Yue; Lv, Jinghua; Yu, Kai; Wang, Chunmei; Su, Zhanhua; Wang, Lu; Zhou, Baibin; New J. Chem. 41 (2017) 12459–12469; doi:10.1039/C7NJ02615C

data_7056593
_publ_section_title
;
 Synthesis and photo-/electro-catalytic properties of Keggin
 polyoxometalate inorganic-organic hybrid layers based on d10 metal and
 rigid benzo-diazole/-triazole ligands
;
_journal_issue                   21
_journal_name_full               'New J. Chem.'
_journal_page_first              12459
_journal_page_last               12469
_journal_paper_doi               10.1039/C7NJ02615C
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'Mo12 O40 Si, 4(C7 H7 N2)'
_chemical_formula_sum            'C28 H28 Mo12 N8 O40 Si'
_chemical_formula_weight         2295.95
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-02-18 deposited with the CCDC.
2017-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                69.701(3)
_cell_angle_beta                 82.052(3)
_cell_angle_gamma                71.665(2)
_cell_formula_units_Z            1
_cell_length_a                   9.9145(16)
_cell_length_b                   11.2727(19)
_cell_length_c                   13.766(2)
_cell_measurement_reflns_used    7650
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.04
_cell_measurement_theta_min      2.12
_cell_volume                     1369.0(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71068
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0913
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7650
_diffrn_reflns_theta_full        27.04
_diffrn_reflns_theta_max         27.04
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    2.784
_exptl_absorpt_correction_T_max  0.596
_exptl_absorpt_correction_T_min  0.532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.785
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1090
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.866
_refine_diff_density_min         -2.828
_refine_diff_density_rms         0.317
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         5868
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0722
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                3522
_reflns_number_total             5868
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7nj02615c2.cif
_cod_data_source_block           test_0m_CCDC1
_cod_database_code               7056593