In situ ligand-induced Ln-MOFs based on a chromophore moiety: white light emission and turn-on detection of trace antibiotics
Feng, Xun; Shang, Yapei; Zhang, Ka; Hong, Manzhou; Li, Junfeng; Xu, Hongdi; Wang, Liya; Li, Zhongjun; CrystEngComm  (2022) –; doi:10.1039/D2CE00613H

data_7245017
_publ_section_title
;
 &#x000D; In situ ligand-induced Ln-MOFs based on a chromophore moiety:
 white light emission and turn-on detection of trace antibiotics
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00613H
_journal_year                    2022
_chemical_formula_moiety         'C34 H23 Gd2 N3 O18'
_chemical_formula_sum            'C34 H22 Gd2 N3 O18'
_chemical_formula_weight         1075.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-08-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2021-10-21 deposited with the CCDC.	2022-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.005(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.5877(12)
_cell_length_b                   31.5073(11)
_cell_length_c                   17.9802(7)
_cell_measurement_reflns_used    4232
_cell_measurement_temperature    293.7(3)
_cell_measurement_theta_max      22.2950
_cell_measurement_theta_min      3.5100
_cell_volume                     9528.0(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.7(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.970
_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    -28.00  45.00   1.00   17.50    --  -13.80  57.00 -90.00   73
  2  \w    -18.00  52.00   1.00   17.50    --  -13.80  57.00 150.00   70
  3  \w    -20.00  14.00   1.00   17.50    --  -13.80 -99.00 -60.00   34
  4  \w     25.00  70.00   1.00   17.50    --   14.74  38.00-120.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0344144000
_diffrn_orient_matrix_UB_12      0.0112048000
_diffrn_orient_matrix_UB_13      0.0016356000
_diffrn_orient_matrix_UB_21      0.0223613000
_diffrn_orient_matrix_UB_22      0.0190803000
_diffrn_orient_matrix_UB_23      0.0079182000
_diffrn_orient_matrix_UB_31      -0.0095814000
_diffrn_orient_matrix_UB_32      0.0041893000
_diffrn_orient_matrix_UB_33      -0.0404657000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0893
_diffrn_reflns_av_unetI/netI     0.1680
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_number            9462
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.453
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.825
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       block
_exptl_crystal_F_000             4152
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.971
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         9462
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0703
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0419P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1423
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5586
_reflns_number_total             9462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00613h2.cif
_cod_data_source_block           sypl71-gd-porous_sq_s
_cod_original_cell_volume        9527.9(9)
_cod_database_code               7245017
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.827
_shelx_estimated_absorpt_t_min   0.728
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Rotating group:
 O15(H15A,H15B), O16(H16A,H16B), O17(H17A,H17B), O18(H18A,H18B)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C5(H5), C3(H3), C20(H20), C23(H23), C30(H30), C28(H28),
 N3(H3A), C25(H25), C31(H31), C27(H27), C26(H26), C33(H33), C32(H32)
;
_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 1.369
_oxdiff_exptl_absorpt_empirical_full_min 0.722