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_4132028
_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            'C164 H120 B4 F16 N40 O24 Pd4 S3'
_chemical_formula_weight         3904.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                90
_cell_angle_beta                 96.009(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.7178(4)
_cell_length_b                   34.1498(6)
_cell_length_c                   18.9986(3)
_cell_measurement_reflns_used    14630
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.3780
_cell_measurement_theta_min      3.5530
_cell_volume                     10786.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    shelxs
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3503
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44001
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.399
_diffrn_reflns_theta_min         3.352
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.518
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       block
_exptl_crystal_F_000             3944
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.827
_refine_diff_density_min         -1.233
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.630
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     932
_refine_ls_number_reflns         21696
_refine_ls_number_restraints     1027
_refine_ls_restrained_S_all      1.618
_refine_ls_R_factor_all          0.1375
_refine_ls_R_factor_gt           0.1186
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3659
_refine_ls_wR_factor_ref         0.3949
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16982
_reflns_number_total             21696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b00394_si_003.cif
_cod_data_source_block           clx-0321dbt_sq
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4132028
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.620
_shelx_estimated_absorpt_t_max   0.620
_shelx_res_checksum              2600
_shelx_hkl_checksum              97819
_shelx_fab_checksum              41705