A highly stable Eu-MOF multifunctional luminescent sensor for the effective detection of Fe3+, Cr2O72−/CrO42− and aspartic acid in aqueous systems
Sun, Yin-Xia; Guo, Geng; Ding, Wen-Min; Han, Wen-Yu; Li, Juan; Deng, Zhe-Peng; CrystEngComm 24 (2022) 1358–1367; doi:10.1039/D1CE01432C

data_7244279
_publ_section_title
;
 A highly stable Eu-MOF multifunctional luminescent sensor for the
 effective detection of Fe3+, Cr2O72&#x2212;/CrO42&#x2212; and aspartic
 acid in aqueous systems
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1358
_journal_page_last               1367
_journal_paper_doi               10.1039/D1CE01432C
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         '0.5(C784 H400 Eu32 N96 O224), 4(C4 H12 N)'
_chemical_formula_sum            'C408 H248 Eu16 N52 O112'
_chemical_formula_weight         10101.93
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-22 deposited with the CCDC.	2021-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.3041(9)
_cell_length_b                   28.6028(14)
_cell_length_c                   29.0127(13)
_cell_measurement_reflns_used    4183
_cell_measurement_temperature    292.4(3)
_cell_measurement_theta_max      69.2480
_cell_measurement_theta_min      7.6510
_cell_volume                     18508.9(14)
_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)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.4(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.965
_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     65.00 130.00   1.00   26.00    --  108.00 -50.00   0.00   65
  2  \w     64.00 110.00   1.00   19.00    --   54.00-125.00 120.00   46
  3  \w     43.00 111.00   1.00   26.00    --  108.00-111.00  60.00   68
  4  \w     37.00  90.00   1.00   26.00    --  108.00 -98.00-106.00   53
  5  \w     33.00  64.00   1.00    8.00    --    0.00  57.00-180.00   31
  6  \w     86.00 127.00   1.00   26.00    --  108.00  50.00  60.00   41
  7  \w    143.00 174.00   1.00   26.00    --  108.00  50.00  60.00   31
  8  \w     34.00 122.00   1.00   19.00    --   54.00  57.00-180.00   88
  9  \w    -12.00  32.00   1.00    8.00    --    0.00  57.00-180.00   44
 10  \w     22.00  60.00   1.00    8.00    --    0.00  57.00 -90.00   38
 11  \w     46.00  80.00   1.00   19.00    --   54.00-125.00-150.00   34
 12  \w     61.00 121.00   1.00   19.00    --   54.00  57.00  60.00   60
 13  \w    102.00 128.00   1.00   26.00    --  108.00 111.00 -60.00   26
 14  \w     72.00 122.00   1.00   26.00    --  108.00 178.00  90.00   50
;
_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      0.0001750000
_diffrn_orient_matrix_UB_12      0.0528305500
_diffrn_orient_matrix_UB_13      -0.0102863500
_diffrn_orient_matrix_UB_21      0.0272309000
_diffrn_orient_matrix_UB_22      -0.0097377500
_diffrn_orient_matrix_UB_23      -0.0478137500
_diffrn_orient_matrix_UB_31      -0.0634666000
_diffrn_orient_matrix_UB_32      -0.0040305500
_diffrn_orient_matrix_UB_33      -0.0207339500
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            12214
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.841
_diffrn_reflns_theta_min         5.002
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.881
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78661
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.813
_exptl_crystal_description       block
_exptl_crystal_F_000             9928
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.932
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         4237
_refine_ls_number_restraints     546
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0317P)^2^+199.6358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0946
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3698
_reflns_number_total             4237
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01432c2.cif
_cod_data_source_block           syx_g3
_cod_depositor_comments          'Adding full bibliography for 7244279.cif.'
_cod_original_cell_volume        18509.0(15)
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               7244279
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.692
_shelx_estimated_absorpt_t_min   0.436
_reflns_odcompleteness_completeness 98.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C17 \\sim C4 \\sim C19 \\sim C2 \\sim C23 \\sim C16 \\sim C24 \\sim C9 \\sim
C20 \\sim C12 \\sim C15 \\sim C11 \\sim C3 \\sim C22 \\sim C8 \\sim C13 \\sim
C10 \\sim C18 \\sim C5 \\sim C7 \\sim C21 \\sim C1 \\sim C6 \\sim C14 \\sim C25
\\sim C26 \\sim Eu1: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N4) \\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(C25) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
Uanis(O7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
3.a Riding coordinates:
 N4(H26A,H26B,H26C)
3.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C9(H9), C20(H20), C12(H12), C15(H15), C11(H11), C8(H8), C18(H18),
 C5(H5), C21(H21), C6(H6), C14(H14), C25(H25)
;
_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 1.323
_oxdiff_exptl_absorpt_empirical_full_min 0.729