Water-Soluble Redox-Active Cage Hosting Polyoxometalates for Selective Desulfurization Catalysis.
Cai, Li-Xuan; Li, Shao-Chuan; Yan, Dan-Ni; Zhou, Li-Peng; Guo, Fang; Sun, Qing-Fu; Journal of the American Chemical Society 140 (2018) 4869–4876; doi:10.1021/jacs.8b00394

data_4132029
_publ_section_title
;
 Water-Soluble Redox-Active Cage Hosting Polyoxometalates for Selective
 Desulfurization Catalysis.
;
_journal_issue                   14
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4869
_journal_page_last               4876
_journal_paper_doi               10.1021/jacs.8b00394
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C128 H96 B4 F16 N40 O24 Pd4'
_chemical_formula_weight         3351.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                90
_cell_angle_beta                 90.18(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.388(4)
_cell_length_b                   36.235(7)
_cell_length_c                   38.605(8)
_cell_measurement_reflns_used    204514
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.000
_cell_measurement_theta_min      1.089
_cell_volume                     25722(9)
_computing_cell_refinement       ApexIII
_computing_data_reduction        ApexIII
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement.details
' 1.00 degrees, 5.3 sec, detector distance 200.01 mm'
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68857
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.937
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            48818
_diffrn_reflns_point_group_measured_fraction_full 0.937
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        20.000
_diffrn_reflns_theta_max         20.000
_diffrn_reflns_theta_min         1.089
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.302
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    0.865
_exptl_crystal_description       block
_exptl_crystal_F_000             6736
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.407
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.539
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1945
_refine_ls_number_reflns         24767
_refine_ls_number_restraints     2729
_refine_ls_restrained_S_all      1.594
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0989
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3273
_refine_ls_wR_factor_ref         0.3407
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20122
_reflns_number_total             24767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b00394_si_002.cif
_cod_data_source_block           p21n_sq
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4132029
_shelx_shelxl_version_number     2016/4
_shelx_res_checksum              61063
_shelx_hkl_checksum              42444
_shelx_fab_checksum              62066