A cucurbit[6]uril-based supramolecular assembly as a highly sensitive and quickly responsive luminescent sensor for the detection of fluoroquinolones antibiotics in simulated wastewater
Liu, Mei; Shi, Lulu; Li, Hui; CrystEngComm  (2020) –; doi:10.1039/D0CE00603C

data_7240512
_publ_section_title
;
 A cucurbit[6]uril-based supramolecular assembly as a highly sensitive and
 quickly responsive luminescent sensor for the detection of
 fluoroquinolones antibiotics in simulated wastewater
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00603C
_journal_year                    2020
_chemical_formula_moiety
'2(C12 H8 O6 S2), C39 H63 N25 Na4 O23, 2(H2 O)'
_chemical_formula_sum            'C63 H83 N25 Na4 O37 S4'
_chemical_formula_weight         2002.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-05-10
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-10 deposited with the CCDC.	2020-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.691(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.2749(9)
_cell_length_b                   24.769(2)
_cell_length_c                   14.9058(12)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    273
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.84
_cell_volume                     4158.1(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_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  0.0531
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            47673
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.736
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.243
_exptl_absorpt_correction_T_max  0.7856
_exptl_absorpt_correction_T_min  0.5612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker;sadabs;2018
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       block
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.151
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         7338
_refine_ls_number_restraints     825
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0927
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1130P)^2^+14.5232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2203
_refine_ls_wR_factor_ref         0.2325
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6257
_reflns_number_total             7338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00603c2.cif
_cod_data_source_block           mo_20190721_shilulu_liumei_2_0
_cod_original_cell_volume        4158.2(6)
_cod_database_code               7240512
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.955
_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, All O(H,H) groups, All O(H,H,H,H) groups
2. Restrained distances
 O3-C0AA
 1.2 with sigma of 0.01
 C0AA-C1AA
 2.5 with sigma of 0.01
 O3-N0AA
 2.3 with sigma of 0.01
 N0AA-C0AA = N0AA-C1AA
 1.5 with sigma of 0.01
 C2AA-C1AA
 2.5 with sigma of 0.01
 C0AA-C2AA
 2.5 with sigma of 0.01
 N0AA-C2AA = N0AA-C1AA
 1.48 with sigma of 0.01
 N0AA-C0AA
 1.48 with sigma of 0.01
 O10-H10B = O10-H10A
 0.84 with sigma of 0.02
 H10B-H10A
 1.46 with sigma of 0.02
 H10B-Na2
 2.4 with sigma of 0.02
 H10A-Na2
 2.5 with sigma of 0.02
 Na2-O10
 2.3 with sigma of 0.02
 S002-O15 \\sim S002-O19 \\sim S002-O20 \\sim S002-O18 \\sim S002-O17 \\sim
S002-O16
 with sigma of 0.02
3. Restrained planarity
 C1AA, C2AA, N0AA, C0AA, O3
 with sigma of 0.01
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C0AA \\sim O3 \\sim N0AA \\sim C1AA \\sim C2AA: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
Uanis(O15) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O17)
\\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O19) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(Na3) \\sim Ueq, Uanis(Na2) \\sim Ueq, Uanis(O15) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(O15) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O3) \\sim Ueq, Uanis(N0AA) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C2AA)
\\sim Ueq, Uanis(C1AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
6. Rigid body (RIGU) restrains
 O3, C0AA, N0AA, C1AA, C2AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
7. Others
 Fixed Sof: H11A(0.5) H11B(0.5) H11C(0.5) H11D(0.5) Na3(0.5) O19(0.75)
 O15(0.75) O17(0.75) O14(0.5) H14A(0.5) H14B(0.5) O12(0.5) H12C(0.5) H12D(0.5)
 O3(0.5) O20(0.25) O16(0.25) O18(0.25) Na2(0.5) N0AA(0.5) C0AA(0.5) H0AA(0.5)
 C1AA(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C2AA(0.5) H2AA(0.5) H2AB(0.5) H2AC(0.5)
 Fixed Z: N0AA(-0.01263)
8.a Riding coordinates:
 O11(H11A,H11B), O11(H11C,H11D), C2AA(H2AA,H2AB,H2AC)
8.b Free rotating group:
 O13(H13A,H13B)
8.c Rotating group:
 O2(H2A,H2B), O1(H1A,H1B), O14(H14A,H14B), O12(H12C,H12D)
8.d Ternary CH refined with riding coordinates:
 C4(H4), C15(H15), C3(H3), C14(H14), C10(H10), C8(H8)
8.e Secondary CH2 refined with riding coordinates:
 C1(H1C,H1D), C12(H12A,H12B), C6(H6A,H6B), C18(H18A,H18B), C17(H17A,H17B),
 C7(H7A,H7B)
8.f Me refined with riding coordinates:
 C1AA(H1AA,H1AB,H1AC)
8.g Aromatic/amide H refined with riding coordinates:
 C27(H27), C26(H26), C21(H21), C24(H24), C23(H23), C30(H30), C20(H20),
 C29(H29), C0AA(H0AA)
;
_olex2_submission_special_instructions 'No special instructions were received'