Highly pH-stable lanthanide MOFs: tunable luminescence and ratiometric luminescent probe for sulfamethazine
Zhang, Xu; Liu, Dongyan; Yu, Jiahui; Li, Xin; Zheng, Hanwen; Zhou, Yanan; Huang, Cui-Ying; Zhu, Yanyu; Jiao, Cheng–Qi; Sun, Zhen-Gang; Dalton Transactions  (2023) –; doi:10.1039/D3DT01117H

data_7713113
_publ_section_title
;
 Highly pH-stable lanthanide MOFs: tunable luminescence and ratiometric
 luminescent probe for sulfamethazine
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01117H
_journal_year                    2023
_chemical_formula_moiety         'C11 H13 F N O10 P2 Tb, 2(H2 O)'
_chemical_formula_sum            'C11 H17 F N O12 P2 Tb'
_chemical_formula_weight         595.11
_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     direct
_audit_creation_date             2023-05-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-05-16 deposited with the CCDC.	2023-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 125.399(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.0892(16)
_cell_length_b                   8.8694(5)
_cell_length_c                   17.2574(9)
_cell_measurement_reflns_used    5528
_cell_measurement_temperature    296.15(10)
_cell_measurement_theta_max      25.0790
_cell_measurement_theta_min      2.3540
_cell_volume                     3629.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_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    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.15(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.970
_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      0.26 183.26   0.50    4.00    --   27.00  73.75 -25.74  366
  2  \w     -4.74 127.26   0.50    4.00    --   33.00  73.75  62.26  264
  3  \w     -2.74  69.26   0.50    4.00    --   33.00  73.75 154.26  144
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0284103000
_diffrn_orient_matrix_UB_12      0.0338133000
_diffrn_orient_matrix_UB_13      0.0179177000
_diffrn_orient_matrix_UB_21      0.0097890000
_diffrn_orient_matrix_UB_22      0.0506079000
_diffrn_orient_matrix_UB_23      -0.0218957000
_diffrn_orient_matrix_UB_31      -0.0280731000
_diffrn_orient_matrix_UB_32      0.0518159000
_diffrn_orient_matrix_UB_33      0.0097225000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8555
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.044
_diffrn_reflns_theta_max         25.044
_diffrn_reflns_theta_min         2.361
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.148
_exptl_absorpt_correction_T_max  0.04468
_exptl_absorpt_correction_T_min  0.02634
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
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    2.178
_exptl_crystal_description       block
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.042
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         1.455
_refine_diff_density_min         -2.386
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3130
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0750
_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^)+(0.0130P)^2^+352.3873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1536
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2707
_reflns_number_total             3130
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 2.8181\% 
around [-0.01 -0.00 1.00] (reciprocal) or [0.00 -0.02 1.00] (direct)
;
_cod_data_source_file            d3dt01117h2.cif
_cod_data_source_block           szg289
_cod_database_code               7713113
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.845
_shelx_estimated_absorpt_t_min   0.585
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
C8 \\sim C9 \\sim C7 \\sim C4 \\sim C3 \\sim C5 \\sim C6 \\sim C2 \\sim C1
\\sim C10 \\sim C11: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(O3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C7, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Riding coordinates:
 O11(H11A,H11B), O12(H12A,H12B)
4.b Ternary CH refined with riding coordinates:
 N1(H1)
4.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B)
4.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C5(H5), C6(H6A), C8(H8)
4.e Fitted hexagon refined as free rotating group:
 C9(C4,C5,C6,C7,C8)
4.f Idealised tetrahedral OH refined as rotating group:
 O3(H3), O6(H6)
;
_shelx_res_checksum              59227
_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 1.263
_oxdiff_exptl_absorpt_empirical_full_min 0.807
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2