Synthesis of two new copper-sandwiched polyoxotungstates and the influence of nuclear number on catalytic hydrogen evolution activity
Su, Zhao-Min; Zhang, Mo; An, Qingqing; Qin, Dan; Li, Hai-Lou; Lv, Hongjin; Jia, Zhiyu; Zhang, Qiang; Yang, Guo-Yu; New Journal of Chemistry 44 (2020) 11035–11041; doi:10.1039/D0NJ02065F

data_7059678
_publ_section_title
;
 Synthesis of two new copper-sandwiched polyoxotungstates and the
 influence of nuclear number on catalytic hydrogen evolution activity
;
_journal_issue                   26
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11035
_journal_page_last               11041
_journal_paper_doi               10.1039/D0NJ02065F
_journal_volume                  44
_journal_year                    2020
_chemical_formula_sum            'C24 H88 Cu10 N16 O71 Si2 W18'
_chemical_formula_weight         5743.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2020-05-26 deposited with the CCDC.	2020-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.901(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6402(10)
_cell_length_b                   31.703(2)
_cell_length_c                   12.2361(9)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.83
_cell_measurement_theta_min      2.28
_cell_volume                     4799.4(6)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0481
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            63281
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.497
_diffrn_reflns_theta_min         1.767
_exptl_absorpt_coefficient_mu    23.768
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    3.974
_exptl_crystal_description       prism
_exptl_crystal_F_000             5128
_refine_diff_density_max         2.317
_refine_diff_density_min         -3.194
_refine_diff_density_rms         0.342
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         13332
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0033P)^2^+231.8220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11347
_reflns_number_total             13332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj02065f2.cif
_cod_data_source_block           platon_sq
_cod_depositor_comments
;Adding full bibliography for 7059678--7059679.cif.

 Adding full bibliography for 7059678--7059679.cif.
;
_cod_original_cell_volume        4799.5(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7059678
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              14452
_shelx_fab_checksum              38639