Synergistic catalysis for light-driven proton reduction using a polyoxometalate-based Cu‒Ni heterometallic‒organic framework
Sun, Wenlong; He, Cheng; Liu, Tao; Duan, Chunying; Chemical Communications  (2019) –; doi:10.1039/C8CC09285K

data_7123145
_publ_section_title
;
 Synergistic catalysis for light-driven proton reduction using a
 polyoxometalate-based Cu--Ni heterometallic--organic framework
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC09285K
_journal_year                    2019
_chemical_formula_moiety         'C156 H108 Cu4.50 N18 Ni4.50 O92 P2 W18'
_chemical_formula_sum            'C156 H108 Cu4.5 N18 Ni4.5 O92 P2 W18'
_chemical_formula_weight         7627.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           175
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 6'
_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
_audit_update_record
;
2018-10-30 deposited with the CCDC.
2019-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   18.858(5)
_cell_length_b                   18.858(5)
_cell_length_c                   15.577(5)
_cell_measurement_reflns_used    1819
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.32
_cell_measurement_theta_min      2.16
_cell_volume                     4797(2)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.1201
_diffrn_reflns_av_sigmaI/netI    0.0650
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29458
_diffrn_reflns_theta_full        27.36
_diffrn_reflns_theta_max         27.36
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    11.772
_exptl_absorpt_correction_T_max  0.192
_exptl_absorpt_correction_T_min  0.090
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3524.5
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.860
_refine_diff_density_min         -1.845
_refine_diff_density_rms         0.292
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3761
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0641
_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^)+(0.0673P)^2^+199.3158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1606
_refine_ls_wR_factor_ref         0.1826
_reflns_number_gt                2569
_reflns_number_total             3782
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8cc09285k2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P6/m
_cod_original_formula_sum        'C156 H108 Cu4.50 N18 Ni4.50 O92 P2 W18'
_cod_database_code               7123145