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_7711251
_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 N2 O8 Tb, C3 H7 N O'
_chemical_formula_sum            'C21 H24 Br3 N3 O9 Tb'
_chemical_formula_weight         861.08
_chemical_name_systematic        Tb-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             2021-10-01
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2021-10-11 deposited with the CCDC.	2022-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                109.079(3)
_cell_angle_beta                 114.551(3)
_cell_angle_gamma                97.782(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2415(3)
_cell_length_b                   11.5520(3)
_cell_length_c                   12.9279(4)
_cell_measurement_reflns_used    14540
_cell_measurement_temperature    150.04(10)
_cell_measurement_theta_max      29.4260
_cell_measurement_theta_min      1.9150
_cell_volume                     1369.46(9)
_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      150.04(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 0.843
_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    -65.00  38.00   0.50    0.40    --   10.29 -57.00  60.00  206
  2  \w    -17.00  36.00   0.50    0.40    --   10.29  57.00-180.00  106
  3  \w     37.00  86.00   0.50    0.40    --   10.29  57.00-180.00   98
  4  \w    -90.00 -41.00   0.50    0.40    --  -11.46 159.00 -88.00   98
  5  \w    -67.00 -42.00   0.50    0.40    --  -11.46 118.00 118.00   50
  6  \w     -6.00  64.00   0.50    0.40    --  -11.46  57.00 -90.00  140
  7  \w    -87.00  23.00   0.50    0.40    --  -11.46 -77.00 -30.00  220
  8  \w    -87.00   9.00   0.50    0.40    --  -11.46 -57.00 150.00  192
  9  \w    -89.00  23.00   0.50    0.40    --  -11.46 -19.00 -60.00  224
 10  \w    -73.00 -24.00   0.50    0.40    --  -11.46 -57.00-120.00   98
 11  \w     -9.00  16.00   0.50    0.40    --  -11.46 -57.00-120.00   50
 12  \w     21.00  56.00   0.50    0.40    --   10.29 -99.00 -60.00   70
 13  \w    -11.00  18.00   0.50    0.40    --   10.29 -99.00 -60.00   58
 14  \w     48.00  90.00   0.50    0.40    --   10.29-159.00-121.00   84
 15  \w     14.00  65.00   0.50    0.40    --   10.29-118.00  31.00  102
 16  \w    -11.00  56.00   0.50    0.40    --   10.29 -99.00 120.00  134
;
_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      -0.0111142000
_diffrn_orient_matrix_UB_12      0.0608021000
_diffrn_orient_matrix_UB_13      0.0171617000
_diffrn_orient_matrix_UB_21      0.0483161000
_diffrn_orient_matrix_UB_22      0.0178258000
_diffrn_orient_matrix_UB_23      0.0637279000
_diffrn_orient_matrix_UB_31      0.0537207000
_diffrn_orient_matrix_UB_32      0.0259430000
_diffrn_orient_matrix_UB_33      -0.0092386000
_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  0.0588
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31328
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.482
_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    7.011
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49998
_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    2.088
_exptl_crystal_description       block
_exptl_crystal_F_000             826
_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         4.318
_refine_diff_density_min         -1.752
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6425
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0703P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1094
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5384
_reflns_number_total             6425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01844f2.cif
_cod_data_source_block           lws-150k_CCDC1
_cod_original_cell_volume        1369.46(8)
_cod_database_code               7711251
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.541
_shelx_estimated_absorpt_t_min   0.487
_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. Uiso/Uaniso restraints and constraints
N3 \\sim C19 \\sim C20 \\sim C21 \\sim O9A \\sim C19A \\sim N3A \\sim C20A
\\sim C21A \\sim O9: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
3. Others
 Sof(O9A)=Sof(C19A)=Sof(H19A)=Sof(N3A)=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)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C11(H11), C13(H13), C16(H16), C19(H19), C19A(H19A)
4.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              37066
_shelx_hkl_checksum              71367
_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 1.802
_oxdiff_exptl_absorpt_empirical_full_min 0.619