Size-matched supramolecular assembly between an asymmetric Anderson-type polyoxometalate hybrid and α-/γ-cyclodextrins.
Liu, Chun-Yan; Mu, Yun-Jing; Chen, Wu-Ji; Liu, Cheng-Shuai; Lin, Chang-Gen; Song, Yu-Fei; Chemical communications (Cambridge, England) 61 (2025) 17886–17889; doi:10.1039/d5cc04781a

data_7135070
_publ_section_title
;
 Size-matched supramolecular assembly between an asymmetric Anderson-type
 polyoxometalate hybrid and &#x3b1;-/&#x3b3;-cyclodextrins.
;
_journal_issue                   91
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              17886
_journal_page_last               17889
_journal_paper_doi               10.1039/d5cc04781a
_journal_volume                  61
_journal_year                    2025
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C68 H69.5 Al I Mo6 N Na3 O60.25, 34[H2O]'
_chemical_formula_sum            'C68 H137.5 Al I Mo6 N Na3 O94.25'
_chemical_formula_weight         3275.77
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-04-18
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-10-05 deposited with the CCDC.	2025-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.154(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6954(4)
_cell_length_b                   34.3474(11)
_cell_length_c                   25.0640(8)
_cell_measurement_reflns_used    9238
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      56.986
_cell_measurement_theta_min      3.599
_cell_volume                     12211.1(7)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection
'Bruker BIS V6.2.16/2021-10-22 && APEX4 2021.10-0'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            111372
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         57.136
_diffrn_reflns_theta_min         2.710
_diffrn_source_current           2.86
_diffrn_source_power             0.19977099999999998
_diffrn_source_voltage           69.85
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.491
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.4941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0933 before and 0.0683 after correction.
The Ratio of minimum to maximum transmission is 0.6577.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_description       needle
_exptl_crystal_F_000             6630
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.228
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.222(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2733
_refine_ls_number_reflns         47070
_refine_ls_number_restraints     5294
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0616
_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^)+(0.1121P)^2^+1.2496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.1898
_reflns_Friedel_coverage         0.855
_reflns_Friedel_fraction_full    0.917
_reflns_Friedel_fraction_max     0.879
_reflns_number_gt                36542
_reflns_number_total             47070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04781a2.cif
_cod_data_source_block           20240509_3_0m_sx
_cod_depositor_comments
'Adding full bibliography for 7135070--7135071.cif.'
_cod_original_formula_sum        'C68 H137.50 Al I Mo6 N Na3 O94.25'
_cod_database_code               7135070
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.583
_shelx_estimated_absorpt_t_min   0.493
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.778(7)
 0.222(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
3. Restrained distances
 C136-C93 = C135-C134 = C134-C133 = C133-C132 = C132-C131 = C131-C130 = C128-
 C127 = C129-C128 = C127-C126 = C126-C125 = C124-C125 = C101-C102
 1.54 with sigma of 0.01
 O115-C136 = C133-O83 = O119-C130 = O119-C127 = O105-C126 = O104-C125 = O106-
 C124 = O106-C128 = O107-C129 = O103-C124 = O103-C121
 1.42 with sigma of 0.01
 O115-C93 = O104-C124 = C130-C127 = O111-C131 = O105-C125 = C128-C124
 2.39 with sigma of 0.02
 C126-C124 = C127-C129 = C127-C125 = C133-C131 = C128-C126 = C132-C130 = C134-
 C132 = C135-C133
 2.56 with sigma of 0.02
 O109-C130 = C124-C121 = C131-O119 = O105-C127 = O104-C126 = O107-C128 = O110-
 C133 = O106-C125 = O110-C131 = O109-C132
 2.39 with sigma of 0.02
 I2-C40 \\sim I2A-C40
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(Na2A) \\sim Ueq, Uanis(Na2) \\sim Ueq, Uanis(Na2B) \\sim Ueq, Uanis(O126)
\\sim Ueq, Uanis(O37) \\sim Ueq, Uanis(O108) \\sim Ueq, Uanis(O113) \\sim Ueq,
Uanis(O114) \\sim Ueq, Uanis(O117) \\sim Ueq, Uanis(O118) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Same fragment restrains
{Mo9A, Mo13, Mo14, Mo15, Al2, O31A, O32A, O33A, O34A, O35A, O36A, O38A, O39A,
O40A, O41A, O42A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{Mo9, Mo10, Mo11, Mo12, Al2, O31, O32, O33, O34, O35, O36, O38, O39, O40, O41,
O42}
7. Others
 1*[Sof(Na2)+Sof(O126)]+1*[Sof(Na2A)+Sof(O37)]+1*[Sof(Na2B)+Sof(O108)]=1 with
 esd of 0.00001
 Sof(I2A)=Sof(Mo9A)=Sof(Mo13)=Sof(Mo14)=Sof(Mo15)=Sof(O31A)=Sof(O32A)=
 Sof(O33A)=Sof(O34A)=Sof(O35A)=Sof(O36A)=Sof(O38A)=Sof(O39A)=Sof(O40A)=
 Sof(O41A)=Sof(O42A)=1-FVAR(1)
 Sof(I2)=Sof(Mo9)=Sof(Mo10)=Sof(Mo11)=Sof(Mo12)=Sof(O31)=Sof(O32)=Sof(O33)=
 Sof(O34)=Sof(O35)=Sof(O36)=Sof(O38)=Sof(O39)=Sof(O40)=Sof(O41)=Sof(O42)=FVAR(1)
 Sof(Na2)=Sof(O126)=FVAR(2)
 Sof(Na2A)=Sof(O37)=FVAR(3)
 Sof(Na2B)=Sof(O108)=FVAR(4)
 Sof(Na4A)=1-FVAR(5)
 Sof(Na4)=FVAR(5)
 Fixed Sof: O118(0.5) O116(0.5) O113(0.5)
 Fixed Y: I1(0.59779)
8.a Ternary CH refined with riding coordinates:
 C65(H65), C66(H66), C67(H67), C68(H68), C69(H69), C71(H71), C72(H72),
 C73(H73), C74(H74), C75(H75), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81),
  C83(H83), C84(H84), C85(H85), C86(H86), C87(H87), C89(H89), C90(H90),
 C91(H91), C92(H92), C93(H93), C94(H94), C95(H95), C96(H96), C97(H97), C98(H98),
  C100(H100), C101(H101), C102(H102), C103(H103), C104(H104), C106(H106),
 C107(H107), C108(H108), C109(H109), C110(H110), C112(H112), C113(H113),
 C115(H115), C116(H116), C118(H118), C119(H119), C120(H120), C121(H121),
 C122(H122), C124(H124), C125(H125), C126(H126), C127(H127), C128(H128),
 C130(H130), C131(H131), C132(H132), C133(H133), C134(H134)
8.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C16(H16A,H16B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
  C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C48(H48A,H48B), C70(H70A,
 H70B), C76(H76A,H76B), C82(H82A,H82B), C88(H88A,H88B), C99(H99A,H99B),
 C105(H10A,H10B), C111(H11A,H11B), C117(H11C,H11D), C123(H12C,H12D), C129(H12E,
 H12F), C135(H13C,H13D), C136(H13E,H13F)
8.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C6(H6), C7(H7), C9(H9), C10(H10), C18(H18), C19(H19),
 C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C38(H38),
  C39(H39), C41(H41), C42(H42), C50(H50), C51(H51), C53(H53), C54(H54),
 C56(H56), C57(H57), C58(H58), C60(H60), C61(H61)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1368 electrons were 
found in a volume of 3406\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
34[H2O] per Asymmetric Unit 
which account for 1360 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              51287
_shelx_hkl_checksum              78494
_shelx_fab_checksum              32117
_olex2_submission_special_instructions 'No special instructions were received'