A nonconventional host-guest cubic assembly based on γ-cyclodextrin and a Keggin-type polyoxometalate.
Jiang, Zhan-Guo; Mao, Wei-Tao; Huang, Dan-Ping; Wang, Yu; Wang, Xiao-Juan; Zhan, Cai-Hong; Nanoscale 12 (2020) 10166–10171; doi:10.1039/d0nr00973c

data_1557709
_publ_section_title
;
 A nonconventional host-guest cubic assembly based on \g-cyclodextrin and
 a Keggin-type polyoxometalate.
;
_journal_issue                   18
_journal_name_full               Nanoscale
_journal_page_first              10166
_journal_page_last               10171
_journal_paper_doi               10.1039/d0nr00973c
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety
'6(O40 P W12), 2(Cu1 O6), 3(C96 H110 Na0.67 O80), 4(O)'
_chemical_formula_sum            'C288 H330 Cu2 Na2 O496 P6 W72'
_chemical_formula_weight         25323.58
_space_group_crystal_system      cubic
_space_group_IT_number           197
_space_group_name_Hall           'I 2 2 3'
_space_group_name_H-M_alt        'I 2 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-01-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2020-01-19 deposited with the CCDC.	2020-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   41.6063(14)
_cell_length_b                   41.6063(14)
_cell_length_c                   41.6063(14)
_cell_measurement_reflns_used    9721
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      2.40
_cell_volume                     72024(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            268668
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         2.077
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.618
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10'
_exptl_crystal_colour            bluish
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_density_diffrn    2.335
_exptl_crystal_description       block
_exptl_crystal_F_000             46096
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.568
_refine_diff_density_min         -1.305
_refine_diff_density_rms         0.202
_refine_ls_abs_structure_details
;
 Flack x determined using 11715 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.012(3)
_refine_ls_extinction_coef       0.0000046(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1286
_refine_ls_number_reflns         27556
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+972.5737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0939
_reflns_Friedel_coverage         0.920
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                25844
_reflns_number_total             27556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nr00973c2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 1557709--1557710.cif.'
_cod_original_cell_volume        72024(7)
_cod_database_code               1557709
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Same fragment restrains
{O14B, O15B, O21B, C24B, C25B, C26B, C39B} sigma for 1-2: 0.02, 1-3: 0.04
{O138, O114, O99, C206, C29, C30, C31} sigma for 1-2: 0.02, 1-3: 0.04
as
{O14A, O15A, O21A, C24A, C25A, C26A, C39A}
3. Others
 Sof(O14B)=Sof(O15B)=Sof(O21B)=Sof(C24B)=Sof(H24B)=Sof(C25B)=Sof(H25B)=
 Sof(C26B)=Sof(H26B)=Sof(C39B)=Sof(H39B)=1-FVAR(1)
 Sof(O14A)=Sof(O15A)=Sof(O21A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=
 Sof(C26A)=Sof(H26A)=Sof(C39A)=Sof(H39A)=FVAR(1)
 Fixed Sof: Na1(0.33333)
4.a Ternary CH refined with riding coordinates:
 C24A(H24A), C25A(H25A), C26A(H26A), C39A(H39A), C24B(H24B), C25B(H25B),
 C26B(H26B), C39B(H39B), C206(H206), C29(H29), C30(H30), C31(H31), C1(H1),
 C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C23(H23), C32(H32), C35(H35), C36(H36), C37(H37), C40(H40), C182(H182),
 C183(H183), C184(H184), C185(H185), C187(H187), C209(H209), C213(H213)
4.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C12(H12A,H12B), C19(H19A,H19B), C33(H33A,H33B), C34(H34A,H34B),
 C41(H41A,H41B), C208(H20A,H20B), C214(H21A,H21B)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'