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_7245016
_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 N3 O18.5 Sm2'
_chemical_formula_sum            'C34 H31 N3 O22.5 Sm2'
_chemical_formula_weight         1142.32
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-21 deposited with the CCDC.	2022-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.351(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.4522(5)
_cell_length_b                   31.6114(7)
_cell_length_c                   18.0196(3)
_cell_measurement_reflns_used    14803
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.7140
_cell_measurement_theta_min      3.7980
_cell_volume                     9488.8(4)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.826
_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    -16.00  24.00   1.00   12.50    --  -13.80 -99.00  90.00   40
  2  \w    -40.00  29.00   1.00   12.50    --   14.82 -57.00 -30.00   69
  3  \w    -25.00  22.00   1.00   12.50    --   14.82 -57.00  90.00   47
  4  \w      7.00  62.00   1.00   12.50    --   14.82  38.00 -90.00   55
;
_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      0.0276832000
_diffrn_orient_matrix_UB_12      0.0156973000
_diffrn_orient_matrix_UB_13      0.0196412000
_diffrn_orient_matrix_UB_21      -0.0264369000
_diffrn_orient_matrix_UB_22      0.0160764000
_diffrn_orient_matrix_UB_23      -0.0203362000
_diffrn_orient_matrix_UB_31      -0.0185767000
_diffrn_orient_matrix_UB_32      0.0005900000
_diffrn_orient_matrix_UB_33      0.0300196000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.826
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21589
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.826
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.466
_diffrn_reflns_theta_min         3.447
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.529
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85464
_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            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       block
_exptl_crystal_F_000             4480
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         3.318
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         9917
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0564
_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^)+(0.1061P)^2^+150.0892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1809
_refine_ls_wR_factor_ref         0.1913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8226
_reflns_number_total             9917
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00613h2.cif
_cod_data_source_block           l71-sm
_cod_original_formula_sum        'C34 H31 N3 O22.50 Sm2'
_cod_database_code               7245016
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_usercomment     'C H O N Sm'
_shelx_estimated_absorpt_t_max   0.619
_shelx_estimated_absorpt_t_min   0.548
_reflns_odcompleteness_completeness 99.57
_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,H) groups
2. Restrained distances
 Sm1-O17 \\sim Sm1-O17A \\sim Sm1-O16 \\sim Sm1-O15 \\sim Sm1-O15A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O17A) = Uanis(O17)
Uanis(O15A) = Uanis(O15)
4. Others
 Sof(O17A)=Sof(H17C)=Sof(H17D)=1-FVAR(1)
 Sof(O17)=Sof(H17A)=Sof(H17B)=FVAR(1)
 Sof(O15A)=Sof(H15C)=Sof(H15D)=1-FVAR(2)
 Sof(O15)=Sof(H15A)=Sof(H15B)=FVAR(2)
 Fixed Sof: O16(0.5) H16A(0.5) H16B(0.5)
5.a Riding coordinates:
 O15(H15A,H15B), O16(H16A,H16B), O17(H17A,H17B), O18(H18A,H18B), O19(H19A,
 H19B), O17A(H17C,H17D), O15A(H15C,H15D)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C11(H11), C13(H13), C15(H15), C16(H16), C18(H18), C19(H19),
 C20(H20), C21(H21), C23(H23), C24(H24), C28(H28), C30(H30)
;
_shelx_res_checksum              82936
_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 1.266
_oxdiff_exptl_absorpt_empirical_full_min 0.840