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_4127919
_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
'K2.5 Na2.5 (P W12 O40) (C36 H60 O30) (C2 H3 O2) (H O), 19(H2 O)'
_chemical_formula_sum            'C38 H102 K2.5 Na2.5 O92 P W12'
_chemical_formula_weight         4423.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 90.376(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.7418(8)
_cell_length_b                   15.6598(8)
_cell_length_c                   18.4127(9)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      66.40
_cell_measurement_theta_min      2.40
_cell_volume                     4827.2(4)
_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 0.992
_diffrn_measured_fraction_theta_max 0.980
_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  0.0534
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            67495
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        62.381
_diffrn_reflns_theta_max         66.680
_diffrn_reflns_theta_min         2.400
_diffrn_source                   'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    28.061
_exptl_absorpt_correction_T_max  0.1489
_exptl_absorpt_correction_T_min  0.0467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1154 before and 0.0814 after correction.
The Ratio of minimum to maximum transmission is 0.3136.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.043
_exptl_crystal_description       prism
_exptl_crystal_F_000             4088
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         4.120
_refine_diff_density_min         -3.884
_refine_diff_density_rms         0.348
_refine_ls_abs_structure_details
;
 Flack x determined using 6054 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.068(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1308
_refine_ls_number_reflns         16220
_refine_ls_number_restraints     617
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0633
_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^)+(0.1441P)^2^+36.7151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2012
_refine_ls_wR_factor_ref         0.2052
_reflns_Friedel_coverage         0.916
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                14853
_reflns_number_total             16220
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b11998_si_003.cif
_cod_data_source_block           POT-CD
_cod_original_formula_sum        'C38 H102 K2.50 Na2.50 O92 P W12'
_cod_database_code               4127919
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.081
_shelx_estimated_absorpt_t_max   0.134
_shelx_res_checksum              17125
_shelx_hkl_checksum              94858