Polyoxometalate-Cyclodextrin Metal-Organic Frameworks: From Tunable Structure to Customized Storage Functionality.
Yang, Peng; Zhao, Wenli; Shkurenko, Aleksander; Belmabkhout, Youssef; Eddaoudi, Mohamed; Dong, Xiaochen; Alshareef, Husam N.; Khashab, Niveen M.; Journal of the American Chemical Society 141 (2019) 1847–1851; doi:10.1021/jacs.8b11998

data_4127918
_publ_section_title
;
 Polyoxometalate-Cyclodextrin Metal-Organic Frameworks: From Tunable
 Structure to Customized Storage Functionality.
;
_journal_issue                   5
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1847
_journal_page_last               1851
_journal_paper_doi               10.1021/jacs.8b11998
_journal_volume                  141
_journal_year                    2019
_chemical_absolute_configuration syn
_chemical_formula_moiety
'K23 H15 (P10 Pd15.5 O50)2 (C48 H80 O40)2, 120 (H2 O)'
_chemical_formula_sum            'C96 H415 K23 O300 P20 Pd31'
_chemical_formula_weight         11188.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5988(8)
_cell_length_b                   47.708(3)
_cell_length_c                   50.646(3)
_cell_measurement_reflns_used    9678
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      70.10
_cell_measurement_theta_min      3.37
_cell_volume                     32858(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection
'Bruker APEX2 v2009.3-0 (Bruker AXS Inc., 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2009'
_computing_publication_material
'PublCIF. Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker X8 PROSPECTOR APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_unetI/netI     0.0713
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            127994
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        57.901
_diffrn_reflns_theta_max         57.901
_diffrn_reflns_theta_min         1.975
_diffrn_source                   'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    18.079
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.4677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1130 before and 0.0706 after correction.
The Ratio of minimum to maximum transmission is 0.6209.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.262
_exptl_crystal_description       prism
_exptl_crystal_F_000             22216
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.160
_refine_diff_density_max         4.069
_refine_diff_density_min         -1.862
_refine_diff_density_rms         0.247
_refine_ls_abs_structure_details
;
 Flack x determined using 14585 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.116(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3713
_refine_ls_number_reflns         43246
_refine_ls_number_restraints     3042
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0772
_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^)+(0.1387P)^2^+305.2558P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2160
_refine_ls_wR_factor_ref         0.2218
_reflns_Friedel_coverage         0.822
_reflns_Friedel_fraction_full    0.926
_reflns_Friedel_fraction_max     0.926
_reflns_number_gt                39444
_reflns_number_total             43246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b11998_si_002.cif
_cod_data_source_block           POP-CD
_cod_database_code               4127918
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.068
_shelx_estimated_absorpt_t_max   0.160
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              93278
_shelx_hkl_checksum              36540
_shelx_fab_checksum              32623