Design of “turn-off” luminescent Ln-MOFs for sensitive detection of cyanide anion
Liu, Weisai; Wang, Fei; Chen, Xiaoyi; Zhi, Wenke; Wang, Xuquan; Xu, Baoqiang; Yang, Bin; Dalton Transactions  (2022) –; doi:10.1039/D2DT01844F

data_7711250
_publ_section_title
;
 Design of &#x201C;turn-off&#x201D; luminescent Ln-MOFs for sensitive
 detection of cyanide anion
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01844F
_journal_year                    2022
_chemical_formula_moiety         'C18 H17 Br3 Eu N2 O8, C3 H7 N O'
_chemical_formula_sum            'C21 H24 Br3 Eu N3 O9'
_chemical_formula_weight         854.12
_chemical_name_systematic        Eu-DBTA
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-29
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6392)
;
_audit_update_record
;
2021-08-30 deposited with the CCDC.	2022-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                108.813(2)
_cell_angle_beta                 114.558(2)
_cell_angle_gamma                98.648(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2941(2)
_cell_length_b                   11.5981(2)
_cell_length_c                   12.9541(3)
_cell_measurement_reflns_used    22416
_cell_measurement_temperature    149.98(10)
_cell_measurement_theta_max      29.4810
_cell_measurement_theta_min      1.9120
_cell_volume                     1378.91(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.64a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.64a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.64a (Rigaku OD, 2020)'
_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_environment      N~2~
_diffrn_ambient_temperature      149.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.844
_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    -15.00  87.00   0.50    0.35    --   10.29  53.00  88.00  204
  2  \w     -3.00  75.00   0.50    0.35    --   10.29  57.00-120.00  156
  3  \w    -60.00  36.00   0.50    0.35    --   10.29 -53.00 -55.00  192
  4  \w     -3.00  56.00   0.50    0.35    --   10.29 -99.00 -60.00  118
  5  \w    -11.00  56.00   0.50    0.35    --   10.29 -99.00  60.00  134
  6  \w    -36.00  62.00   0.50    0.35    --  -11.46  53.00  88.00  196
  7  \w    -67.00 -22.00   0.50    0.35    --  -11.46 117.00  35.49   90
  8  \w    -36.00  62.00   0.50    0.35    --  -11.46  57.00 150.00  196
  9  \w    -11.00  34.00   0.50    0.35    --  -11.46 -99.00 150.00   90
 10  \w     -5.00  33.00   0.50    0.35    --  -11.46 -99.00  90.00   76
 11  \w    -87.00   7.00   0.50    0.35    --  -11.46 -57.00  30.00  188
 12  \w    -86.00 -24.00   0.50    0.35    --  -11.46 -53.00 -55.00  124
;
_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      0.0666737000
_diffrn_orient_matrix_UB_12      0.0468746000
_diffrn_orient_matrix_UB_13      0.0411791000
_diffrn_orient_matrix_UB_21      0.0270721000
_diffrn_orient_matrix_UB_22      -0.0483201000
_diffrn_orient_matrix_UB_23      0.0125759000
_diffrn_orient_matrix_UB_31      0.0131667000
_diffrn_orient_matrix_UB_32      -0.0123869000
_diffrn_orient_matrix_UB_33      -0.0508293000
_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  0.0364
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.844
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30072
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.442
_diffrn_reflns_theta_min         1.913
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.673
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.64a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.057
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: N,N-Dimethylformamide?DMF?'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6452
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0233
_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^)+(0.0176P)^2^+0.8472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0464
_refine_ls_wR_factor_ref         0.0481
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5641
_reflns_number_total             6452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01844f2.cif
_cod_data_source_block           lws-150k
_cod_original_cell_volume        1378.90(5)
_cod_database_code               7711250
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.555
_shelx_estimated_absorpt_t_min   0.501
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O9-C19 = O9A-C19A
 1.21 with sigma of 0.01
 N3-C19 = N3A-C19A
 1.4 with sigma of 0.01
 N3-C21 = N3-C20 = N3A-C20A = N3A-C21A
 1.47 with sigma of 0.01
 N3-O9 = N3A-O9A
 2.262 with sigma of 0.02
 C20-C21 = C21A-C20A
 2.546 with sigma of 0.02
 C21-C19 = C21A-C19A
 2.486 with sigma of 0.02
 C19-C20 = C20A-C21A
 2.486 with sigma of 0.02
3. Restrained planarity
 N3A, C19A, C21A, C20A
 with sigma of 0.1
 N3, C19, C20, C21
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C19A \\sim N3A \\sim C20A \\sim C21A \\sim O9A \\sim C21 \\sim O9 \\sim C19
\\sim N3 \\sim C20: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C20A) \\sim Ueq, Uanis(O9)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C17) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
5. Rigid body (RIGU) restrains
 O9A, N3A, C19A, C20A, C21A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O9, C19, N3, C20, C21
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
6. Others
 Sof(N3A)=Sof(O9A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=
 Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(O9)=Sof(N3)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C11(H11), C13(H13), C16(H16), C19(H19), C19A(H19A)
7.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C20A(H20D,H20E,H20F),
 C21A(H21D,H21E,H21F)
;
_shelx_res_checksum              87500
_shelx_hkl_checksum              18937
_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 1.246
_oxdiff_exptl_absorpt_empirical_full_min 0.874