An unprecedented {Ni14SiW9} hybrid polyoxometalate with high photocatalytic hydrogen evolution activity
Paille, Grégoire; Boulmier, Amandine; Bensaid, Alexandre; Ha-Thi, Minh-Huong; Tran, Thu-Trang; Pino, Thomas; Marrot, Jérôme; Rivière, Eric; Hendon, Christopher H.; Oms, Olivier; Gomez-Mingot, Maria; Fontecave, Marc; Mellot-Draznieks, Caroline; Dolbecq, Anne; Mialane, Pierre; Chemical Communications  (2019) –; doi:10.1039/C9CC01269A

data_7123163
_publ_section_title
;
 An unprecedented {Ni14SiW9} hybrid polyoxometalate with high
 photocatalytic hydrogen evolution activity
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC01269A
_journal_year                    2019
_chemical_formula_sum            'C28 H210 N7 Na12 Ni14 O134 P14 Si W9'
_chemical_formula_weight         6004.16
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-02-26 deposited with the CCDC.    2019-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                111.942(6)
_cell_angle_beta                 90.443(7)
_cell_angle_gamma                98.293(7)
_cell_formula_units_Z            2
_cell_length_a                   15.2253(17)
_cell_length_b                   23.007(2)
_cell_length_c                   29.976(3)
_cell_measurement_reflns_used    9564
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      2.24
_cell_volume                     9616.0(17)
_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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0656
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            266718
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.194
_diffrn_reflns_theta_max         25.194
_diffrn_reflns_theta_min         2.239
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.942
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2014/5)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.074
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             5826
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.180
_platon_squeeze_details          'Spek, A. L. (2015). Acta Cryst. C71, 9-18'
_refine_diff_density_max         5.349
_refine_diff_density_min         -5.909
_refine_diff_density_rms         0.372
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1772
_refine_ls_number_reflns         34100
_refine_ls_number_restraints     911
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1308
_refine_ls_R_factor_gt           0.0987
_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^)+(0.0935P)^2^+832.5519P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2466
_refine_ls_wR_factor_ref         0.2782
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25967
_reflns_number_total             34100
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01269a2.cif
_cod_data_source_block           wid2598_a_sq
_cod_original_cell_volume        9616.2(18)
_cod_database_code               7123163
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.230
_shelx_estimated_absorpt_t_max   0.368
_exptl_absorpt_special_details   'Blessing, Acta Cryst. (1995) A51, 33-38'
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              70674
_shelx_fab_checksum              91596