A turn-on fluorescent Zn(II) metal−organic framework sensor for quantitative anthrax biomarker detection
Hong, Chao; Li, Ling; Zou, Ji-Yong; Zhang, Li; You, Shengyong; Dalton Transactions  (2023) –; doi:10.1039/D3DT00619K

data_7712713
_publ_section_title
;
 A turn-on fluorescent Zn(II) metal&#x2212;organic framework sensor for
 quantitative anthrax biomarker detection
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00619K
_journal_year                    2023
_chemical_formula_moiety         '1.5(C36 H22 N2 O8 Zn2), 0.8(C12 H8 O4), H2 O'
_chemical_formula_sum            'C63.6 H41.4 N3 O16.2 Zn3'
_chemical_formula_weight         1302.90
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-06
_audit_creation_method
;
  Olex2 1.2
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_audit_update_record
;
2022-11-23 deposited with the CCDC.	2023-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                97.934(2)
_cell_angle_beta                 95.154(2)
_cell_angle_gamma                92.056(2)
_cell_formula_units_Z            2
_cell_length_a                   13.1143(3)
_cell_length_b                   13.1651(3)
_cell_length_c                   16.3159(4)
_cell_measurement_reflns_used    17284
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.1130
_cell_measurement_theta_min      1.5650
_cell_volume                     2775.38(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.8060
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -4.00  21.00   0.50    0.78    --   10.52 -99.00-120.00   50
  2  \w    -14.00  12.00   0.50    0.78    --   10.52 -98.00 105.00   52
  3  \w     -6.00  47.00   0.50    0.78    --   10.52  57.00 120.00  106
  4  \w    -38.00   8.00   0.50    0.78    --  -11.30  98.00-148.00   92
  5  \w    -38.00  50.00   0.50    0.78    --  -11.30  57.00 -60.00  176
  6  \w    -37.00  59.00   0.50    0.78    --  -11.30  57.00   0.00  192
  7  \w    -26.00   4.00   0.50    0.78    --  -11.30  19.00 150.00   60
  8  \w     25.00  52.00   0.50    0.78    --  -11.30  19.00 150.00   54
  9  \w    -87.00  14.00   0.50    0.78    --  -11.30 -57.00 150.00  202
 10  \w     -9.00  15.00   0.50    0.78    --  -11.30 -98.00 105.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0188057000
_diffrn_orient_matrix_UB_12      -0.0164593000
_diffrn_orient_matrix_UB_13      -0.0388270000
_diffrn_orient_matrix_UB_21      0.0180647000
_diffrn_orient_matrix_UB_22      -0.0446785000
_diffrn_orient_matrix_UB_23      0.0151791000
_diffrn_orient_matrix_UB_31      -0.0477096000
_diffrn_orient_matrix_UB_32      -0.0264421000
_diffrn_orient_matrix_UB_33      -0.0143694000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.806
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34375
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.806
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.468
_diffrn_reflns_theta_min         1.561
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.364
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_description       block
_exptl_crystal_F_000             1327
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.793
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     899
_refine_ls_number_reflns         12411
_refine_ls_number_restraints     699
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0665P)^2^+7.7342P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1378
_refine_ls_wR_factor_ref         0.1497
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9042
_reflns_number_total             12411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00619k2.cif
_cod_data_source_block           nhc-1234mixed-4-lightyellow-block-100k_auto
_cod_original_formula_sum        'C63.60 H41.40 N3 O16.20 Zn3'
_cod_database_code               7712713
_diffrn_oxdiff_digest_frames
;
01a367c04c088b997e762cd8e04e3e7a5b000300978
;
_diffrn_oxdiff_digest_hkl
;
01653e31588a097837263f64386461128010c9
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 C66-C63 = C65-C56
 1.5 with sigma of 0.01
 O13-C65 = C65-O14
 1.25 with sigma of 0.02
 O15-C66 = C66-O16
 1.25 with sigma of 0.01
 C65A-C56A = C66A-C63A
 1.5 with sigma of 0.01
 O13A-C65A = C65A-O14A
 1.25 with sigma of 0.01
 O15A-C66A = C66A-O16A
 1.25 with sigma of 0.01
 O14-C65 = C65-O13
 1.25 with sigma of 0.01
 O15-O16
 2.165 with sigma of 0.02
 O13-O14
 2.165 with sigma of 0.02
 O15A-O16A
 2.165 with sigma of 0.02
 O13A-O14A
 2.165 with sigma of 0.02
 O14-O13
 2.165 with sigma of 0.04
 C56-O13
 2.385 with sigma of 0.02
 C56-O14
 2.385 with sigma of 0.02
 C63A-O16A
 2.385 with sigma of 0.02
 C63A-O15A
 2.385 with sigma of 0.02
 C56A-O14A
 2.385 with sigma of 0.02
 C63-O16
 2.385 with sigma of 0.02
 C56A-O13A
 2.385 with sigma of 0.02
 C63-O15
 2.385 with sigma of 0.02
 O14-C56 \\sim O13-C56
 with sigma of 0.02
 C66-C62 \\sim C66-C64
 with sigma of 0.02
 O15-C63 \\sim O16-C63
 with sigma of 0.02
 C65-C55 \\sim C65-C57
 with sigma of 0.02
 O15A-C63A \\sim O16A-C63A
 with sigma of 0.02
 C66A-C62A \\sim C66A-C64A
 with sigma of 0.02
 C65A-C55A \\sim C65A-C57A
 with sigma of 0.02
 O14A-C56A \\sim O13A-C56A
 with sigma of 0.02
3. Restrained planarity
 O16, O15, C66, C63
 with sigma of 0.1
 C63, C58, C64, C55, C57, C59, C61, C56, C60, C62, C66, C65
 with sigma of 0.1
 C56, C65, O14, O13
 with sigma of 0.1
 C56A, C55A, C57A, C60A, C58A, C59A, C61A, C64A, C62A, C63A, C66A, C65A
 with sigma of 0.1
 O13A, C65A, O14A, C56A
 with sigma of 0.1
 O16A, C63A, C66A, O15A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C60 \\sim O13 \\sim C65 \\sim O14 \\sim C56 \\sim C55 \\sim C57 \\sim C58 \\sim
C59 \\sim C61 \\sim C64 \\sim C62 \\sim C63 \\sim C66 \\sim O15 \\sim O16:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C66A \\sim O16A \\sim C63A \\sim O15A \\sim C64A \\sim C62A \\sim C59A \\sim
C61A \\sim C60A \\sim C58A \\sim C55A \\sim C57A \\sim C56A \\sim C65A \\sim
O13A \\sim O14A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C60A) \\sim Ueq, Uanis(O16A) \\sim Ueq, Uanis(C66A) \\sim Ueq,
Uanis(C63A) \\sim Ueq, Uanis(O15A) \\sim Ueq, Uanis(C62A) \\sim Ueq,
Uanis(C64A) \\sim Ueq, Uanis(C61A) \\sim Ueq, Uanis(C59A) \\sim Ueq,
Uanis(C58A) \\sim Ueq, Uanis(C55A) \\sim Ueq, Uanis(C57A) \\sim Ueq,
Uanis(C56A) \\sim Ueq, Uanis(C65A) \\sim Ueq, Uanis(O13A) \\sim Ueq,
Uanis(O14A) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(C65)
\\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(C55) \\sim Ueq,
Uanis(C60) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C61)
\\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq,
Uanis(C66) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O15) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C66A) \\sim Ueq, Uanis(O16A) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
5. Rigid body (RIGU) restrains
 C60, O13, C65, O14, C56, C55, C57, C58, C59, C61, C64, C62, C63, C66, O15, O16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C66A, O16A, C63A, O15A, C64A, C62A, C59A, C61A, C60A, C58A, C55A, C57A, C56A,
 C65A, O13A, O14A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Fixed Sof: O13(0.5) H13A(0.5) O14(0.5) O15(0.5) O16(0.5) H16A(0.5) C55(0.5)
 H55(0.5) C56(0.5) C57(0.5) H57(0.5) C58(0.5) H58(0.5) C59(0.5) C60(0.5)
 C61(0.5) H61(0.5) C62(0.5) H62(0.5) C63(0.5) C64(0.5) H64(0.5) C65(0.5)
 C66(0.5) O16A(0.3) H16B(0.3) O13A(0.3) C65A(0.3) O14A(0.3) H14A(0.3) C55A(0.3)
 H55A(0.3) C56A(0.3) C57A(0.3) H57A(0.3) C58A(0.3) H58A(0.3) C59A(0.3)
 C60A(0.3) C61A(0.3) H61A(0.3) C62A(0.3) H62A(0.3) C63A(0.3) C64A(0.3)
 H64A(0.3) C66A(0.3) O15A(0.3)
7.a Riding coordinates:
 O13(H13A), O17(H17A,H17B), O16A(H16B), O14A(H14A)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C7(H7), C8(H8), C10(H10), C13(H13), C15(H15),
 C16(H16), C19(H19), C20(H20), C22(H22), C37(H37), C38(H38), C40(H40), C41(H41),
  C42(H42), C43(H43), C45(H45), C46(H46), C47(H47), C48(H48), C27(H27),
 C29(H29), C30(H30), C33(H33), C34(H34), C36(H36), C49(H49), C50(H50), C52(H52),
  C53(H53), C54(H54), C55(H55), C57(H57), C58(H58), C61(H61), C62(H62),
 C64(H64), C55A(H55A), C57A(H57A), C58A(H58A), C61A(H61A), C62A(H62A),
 C64A(H64A)
7.c Naphthalene refined as free rotating group:
 C55(C56,C57,C58,C59,C60,C61,C62,C63,C64), C55A(C56A,C57A,C58A,C59A,C60A,C61A,
 C62A,C63A,C64A)
7.d Idealised tetrahedral OH refined as rotating group:
 O16(H16A)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.575
_oxdiff_exptl_absorpt_empirical_full_min 0.669
_shelx_estimated_absorpt_t_max   0.811
_shelx_estimated_absorpt_t_min   0.763
_shelx_hkl_checksum              94571
_shelx_res_checksum              97276
_shelx_shelxl_version_number     2019/2