A Lanthanide Luminescence Sensor for Detection of 4-nitrophenol in Aqueous Media
Song, Xue-Qin; Song, Fu-Qiang; Zhang, Pei; Li, Juan; Dalton Transactions  (2023) –; doi:10.1039/D3DT02413J

data_7713947
_publ_section_title
;
 A Lanthanide Luminescence Sensor for Detection of 4-nitrophenol in
 Aqueous Media
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02413J
_journal_year                    2023
_chemical_formula_moiety         'C40 H42 N8 O20 Tb2'
_chemical_formula_sum            'C40 H42 N8 O20 Tb2'
_chemical_formula_weight         1272.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-12-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-11 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.222(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0020(5)
_cell_length_b                   15.5597(5)
_cell_length_c                   24.3406(9)
_cell_measurement_reflns_used    4749
_cell_measurement_temperature    173.20(10)
_cell_measurement_theta_max      70.4340
_cell_measurement_theta_min      4.6320
_cell_volume                     5608.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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      N~2~
_diffrn_ambient_temperature      173.20(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_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  12.00   1.00    2.00    --    0.00  57.00  60.00   27
  2  \w     20.00  60.00   1.00    2.00    --    0.00  57.00  60.00   40
  3  \w    -10.00  87.00   1.00    3.00    --   56.00 -38.00   0.00   97
  4  \w     40.00  99.00   1.00    3.00    --   56.00 -99.00  90.00   59
  5  \w     49.00 106.00   1.00    5.00    --  112.00 -50.00 150.00   57
  6  \w     47.00 136.00   1.00    5.00    --  112.00 -38.00   0.00   89
  7  \w     64.00 116.00   1.00    5.00    --  112.00-111.00 -90.00   52
  8  \w     41.00 106.00   1.00    5.00    --  112.00 -38.00-150.00   65
  9  \w     91.00 162.00   1.00    5.00    --  112.00  25.00-180.00   71
 10  \w    104.00 177.00   1.00    5.00    --  112.00 111.00-180.00   73
 11  \w     68.00 148.00   1.00    5.00    --  112.00 178.00 -90.00   80
 12  \w     70.00 125.00   1.00    5.00    --  112.00 178.00 120.00   55
 13  \w     25.00  86.00   1.00    3.00    --   56.00  77.00-150.00   61
 14  \w     35.00 126.00   1.00    3.00    --   56.00  38.00-180.00   91
 15  \w    -21.00  32.00   1.00    2.00    --    0.00 -77.00 150.00   53
 16  \w    -72.00 -29.00   1.00    2.00    --    0.00 -77.00 150.00   43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0775438000
_diffrn_orient_matrix_UB_12      0.0141438000
_diffrn_orient_matrix_UB_13      0.0488791000
_diffrn_orient_matrix_UB_21      -0.0690202000
_diffrn_orient_matrix_UB_22      0.0251841000
_diffrn_orient_matrix_UB_23      0.0376912000
_diffrn_orient_matrix_UB_31      -0.0066901000
_diffrn_orient_matrix_UB_32      -0.0946980000
_diffrn_orient_matrix_UB_33      0.0174166000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0725
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20418
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.077
_diffrn_reflns_theta_min         3.679
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.873
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       block
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         3.649
_refine_diff_density_min         -1.180
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         10602
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0571P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1307
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8024
_reflns_number_total             10602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02413j2.cif
_cod_data_source_block           songfq_s3_sq
_cod_database_code               7713947
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Rigid bond restraints
 N5, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C31(H31A,H31B), C30(H30A,H30B), C32(H32A,H32B), C12(H12A,
 H12B), C13(H13A,H13B), C11(H11A,H11B), C28(H28A,H28B), C8(H8A,H8B), C10(H10A,
 H10B), C9(H9A,H9B), C29(H29A,H29B)
4.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C34(H34), N4(H4), C36(H36), C25(H25), C14(H14), C24(H24), C16(H16),
 C22(H22), C2(H2), C39(H39), C19(H19), C4(H4A), C5(H5), C3(H3), C38(H38),
 C18(H18), C23(H23)
;
_shelx_res_checksum              32026
_shelx_fab_checksum              27866
_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 1.917
_oxdiff_exptl_absorpt_empirical_full_min 0.692