Metal-organic rotaxane frameworks constructed from a cucurbit[8]uril-based ternary complex for the selective detection of antibiotics.
Wu, Weijie; Xu, Yinghao; Wang, Shoujun; Pang, Qingqing; Liu, Simin; Chemical communications (Cambridge, England) 59 (2023) 5890–5893; doi:10.1039/d3cc00950e

data_7131567
_publ_section_title
;
 Metal-organic rotaxane frameworks constructed from a
 cucurbit[8]uril-based ternary complex for the selective detection of
 antibiotics.
;
_journal_issue                   39
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5890
_journal_page_last               5893
_journal_paper_doi               10.1039/d3cc00950e
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C28 H22 N2 O6 Zn, C24 H24 N16 O8, 12[H2O]'
_chemical_formula_sum            'C52 H70 N18 O26 Zn'
_chemical_formula_weight         1428.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-04-04
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-07 deposited with the CCDC.	2023-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.936(3)
_cell_length_b                   18.3877(14)
_cell_length_c                   21.801(3)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      52.48
_cell_measurement_theta_min      2.50
_cell_volume                     6171.5(15)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker SAINT'
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            48025
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        53.118
_diffrn_reflns_theta_max         53.118
_diffrn_reflns_theta_min         2.497
_exptl_absorpt_coefficient_mu    0.921
_exptl_absorpt_correction_T_max  0.7505
_exptl_absorpt_correction_T_min  0.6108
_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            yellow
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       block
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.846
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         10835
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0609
_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^)+(0.1099P)^2^+5.4266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1819
_refine_ls_wR_factor_ref         0.1899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8752
_reflns_number_total             10835
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00950e2.cif
_cod_data_source_block           wust-1
_cod_depositor_comments
'Adding full bibliography for 7131567--7131568.cif.'
_cod_original_cell_volume        6171.4(13)
_cod_database_code               7131567
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C52'-O5' = C52'-O14' = C52-O5 = C52-O14
 1.3 with sigma of 0.02
 Zn1-O14'
 3 with sigma of 0.02
 Zn1-O5'
 2 with sigma of 0.02
 O5-O14 = O5'-O14'
 2.2 with sigma of 0.02
3. Rigid bond restraints
 C14, C15
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C7 \\sim C7' \\sim C8 \\sim C8' \\sim O14 \\sim O14' \\sim C52 \\sim C52':
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.02 within 2A
Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7') \\sim Ueq, Uanis(C8')
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
5. Others
 Sof(C7')=Sof(H7')=Sof(C8')=Sof(H8')=Sof(C52')=Sof(H52')=Sof(O5')=Sof(O14')=1-
 FVAR(1)
 Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8)=Sof(C52)=Sof(H52)=Sof(O5)=Sof(O14)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C48(H48), C30(H30), C33(H33), C37(H37), C38(H38), C43(H43), C44(H44), C50(H50)
6.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C34(H34A,H34B), C35(H35A,H35B), C40(H40A,
 H40B), C41(H41A,H41B), C46(H46A,H46B), C47(H47A,H47B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C7'(H7'), C8(H8), C8'(H8'), C10(H10),
 C11(H11), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C22(H22),
  C23(H23), C24(H24), C26(H26), C52(H52), C52'(H52')
6.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 492 electrons were 
found in a volume of 1398\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
12[H2O] per Formula Unit 
which account for 480 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              56645
_shelx_hkl_checksum              20863
_shelx_fab_checksum              49068
_olex2_submission_special_instructions 'No special instructions were received'