Dye encapsulated zinc-based metal-organic framework as a dual-emission sensor for highly sensitive detection of antibiotics
Wang, Kang; Duan, Yuhan; Chen, Jiajing; Wang, Haiying; Liu, Hui-Yan; Dalton Transactions  (2021) –; doi:10.1039/D1DT03950D

data_7708980
_publ_section_title
;
 Dye encapsulated zinc-based metal-organic framework as a dual-emission
 sensor for highly sensitive detection of antibiotics
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03950D
_journal_year                    2021
_chemical_formula_moiety         'C26 H28 N4 O12 Zn2, 2[C3H7NO]'
_chemical_formula_sum            'C32 H42 N6 O14 Zn2'
_chemical_formula_weight         865.45
_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   mixed
_audit_creation_date             2021-11-04
_audit_creation_method
;

Olex2 1.5-dev
(compiled 2021.10.14 svn.r9718050b for OlexSys, GUI svn.r6396)
;
_audit_update_record
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2021-11-29 deposited with the CCDC.	2021-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.198(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.123(2)
_cell_length_b                   16.278(4)
_cell_length_c                   13.191(3)
_cell_measurement_reflns_used    4747
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.07
_cell_measurement_theta_min      2.45
_cell_volume                     2076.5(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10830
_diffrn_reflns_point_group_measured_fraction_full 0.864
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_min         2.244
_exptl_absorpt_coefficient_mu    1.222
_exptl_absorpt_correction_T_max  0.766
_exptl_absorpt_correction_T_min  0.711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2008'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.308
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.41(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         6646
_refine_ls_number_restraints     372
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0774
_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^)+(0.1797P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2123
_refine_ls_wR_factor_ref         0.2202
_reflns_Friedel_coverage         0.665
_reflns_Friedel_fraction_full    0.721
_reflns_Friedel_fraction_max     0.715
_reflns_number_gt                5797
_reflns_number_total             6646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03950d2.cif
_cod_data_source_block           compound_1
_cod_original_cell_volume        2076.4(8)
_cod_database_code               7708980
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.766
_shelx_estimated_absorpt_t_min   0.711
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.59(3)
 0.41(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N2-C1C
 1.46 with sigma of 0.02
 C1A-O13
 1.22 with sigma of 0.02
 C1A-N2
 1.36 with sigma of 0.02
 N2-C1B
 1.45 with sigma of 0.02
 C1A-C1B
 2.46 with sigma of 0.04
 C1A-C1C
 2.45 with sigma of 0.04
 N4-C18 \\sim N4-C19 \\sim N4-C31
 with sigma of 0.001
 C18-C19 \\sim C19-C31
 with sigma of 0.001
 C19-C31 \\sim C31-C18
 with sigma of 0.001
 C25A-C23A \\sim C23A-C24A
 with sigma of 0.001
 C25-C24 \\sim C25A-C24A
 with sigma of 0.04
 N6-C23 \\sim N6A-C23A
 with sigma of 0.04
 N6-C24 \\sim N6A-C24A
 with sigma of 0.02
 C25-C23 \\sim C25A-C23A
 with sigma of 0.04
 C25-N6 \\sim C25A-N6A
 with sigma of 0.02
 C23A-C24A \\sim C24A-C25A
 with sigma of 0.001
 C23-C24 \\sim C23A-C24A
 with sigma of 0.04
 N6A-C23A \\sim N6A-C25A \\sim N6A-C24A
 with sigma of 0.001
 C24A-C25A \\sim C25A-C23A
 with sigma of 0.001
 O10-C23 \\sim O10-C23A
 with sigma of 0.02
 O10-N6 \\sim O10-N6A
 with sigma of 0.04
 N2-C1B \\sim N2-C1C
 with sigma of 0.02
 Zn1-O13 \\sim Zn1-O13A
 with sigma of 0.02
 N2-C1B \\sim N2A-C1E
 with sigma of 0.02
 C1A-N2 \\sim C20-N2A
 with sigma of 0.02
 N2-C1C \\sim N2A-C1D
 with sigma of 0.02
 O13-N2 \\sim O13A-N2A
 with sigma of 0.04
 C1B-C1C \\sim C1E-C1D
 with sigma of 0.04
 C1A-O13 \\sim C20-O13A
 with sigma of 0.02
 Zn1-C1A \\sim Zn1-C20
 with sigma of 0.04
 C1A-C1B \\sim C20-C1E
 with sigma of 0.04
 C1A-C1C \\sim C20-C1D
 with sigma of 0.04
 C1D-C1E \\sim C1E-C20
 with sigma of 0.001
 C1B-C1C \\sim C1C-C1A
 with sigma of 0.001
 O10-C23A \\sim O10-C23
 with sigma of 0.001
4. Restrained planarity
 O12, C18, N4, C31, C19
 with sigma of 0.0001
 O10, C23A, N6A, C24A, C25A
 with sigma of 0.0001
 C25, C24, N6, C23, O10
 with sigma of 0.0001
 C1A, O13, N2, C1B, C1C
 with sigma of 0.1
 C1A, N2, C1B, C1C, O13
 with sigma of 0.001
5. Uiso/Uaniso restraints and constraints
C1A \\sim O13 \\sim N2 \\sim C1B \\sim C1C: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O10 \\sim O12 \\sim N4 \\sim C18 \\sim C19 \\sim C31 \\sim C25 \\sim N6 \\sim
C23 \\sim C24 \\sim C25A \\sim N6A \\sim C23A \\sim C24A \\sim C1A \\sim O13
\\sim N2 \\sim C1B \\sim O13A \\sim C20 \\sim N2A \\sim C1D \\sim C1E \\sim
C1C: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
6. Rigid body (RIGU) restrains
 O12, N4, C18, C19, C31
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C25, C24, N6, C23, O10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C24A, N6A, C25A, C23A, O10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1A, O13, N2, C1B, C1C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(N6A)=Sof(C23A)=Sof(H23A)=
 Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(1)
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(N6)=Sof(C23)=Sof(H23)=Sof(C24)=
 Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(1)
 Sof(O13A)=Sof(C20)=Sof(H20)=Sof(N2A)=Sof(C1D)=Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=
 Sof(C1E)=Sof(H1EA)=Sof(H1EB)=Sof(H1EC)=1-FVAR(2)
 Sof(C1A)=Sof(H1A)=Sof(O13)=Sof(N2)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=
 Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=FVAR(2)
8.a Riding coordinates:
 C25(H25A,H25B,H25C), C25A(H25D,H25E,H25F), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,
 H1CC), C1E(H1EA,H1EB,H1EC)
8.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C11(H11), C13(H13), C15(H15), N1(H1), C18(H18),
 C23(H23), C23A(H23A), C1A(H1A), C20(H20)
8.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C31(H31A,H31B,H31C), C24(H24A,H24B,H24C), C24A(H24D,H24E,
 H24F), C1D(H1DA,H1DB,H1DC)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 137 electrons were 
found in a volume of 730\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 2[C3H7NO] per Formula Unit 
which account for 160 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              73728
_shelx_hkl_checksum              36431
_shelx_fab_checksum              75071
_olex2_submission_special_instructions 'No special instructions were received'