Bimetallic Lanthanide-Organic Framework Membranes as a Self-Calibrating Luminescent Sensor for Rapidly Detecting Antibiotics in Water.
Dong, Jie; Hou, Sheng-Li; Zhao, Bin; ACS applied materials & interfaces 12 (2020) 38124–38131; doi:10.1021/acsami.0c09940

data_4517961
_publ_section_title
;
 Bimetallic Lanthanide-Organic Framework Membranes as a Self-Calibrating
 Luminescent Sensor for Rapidly Detecting Antibiotics in Water.
;
_journal_issue                   34
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              38124
_journal_page_last               38131
_journal_paper_doi               10.1021/acsami.0c09940
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety         'C84 H64 Eu5 N2 O46, 1.5(O)'
_chemical_formula_sum            'C84 H64 Eu5 N2 O47.5'
_chemical_formula_weight         2621.17
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                98.138(4)
_cell_angle_beta                 108.822(5)
_cell_angle_gamma                105.573(7)
_cell_formula_units_Z            1
_cell_length_a                   12.2976(10)
_cell_length_b                   15.1864(10)
_cell_length_c                   17.2929(7)
_cell_measurement_reflns_used    5625
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      27.7460
_cell_measurement_theta_min      3.1250
_cell_volume                     2850.9(4)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -22.00  29.00   1.00   20.91    --   18.94 -57.00  60.00   51
  2  \w     24.00  61.00   1.00   20.91    --   18.94 -99.00  30.00   37
  3  \w    -48.00  49.00   1.00   20.91    --  -19.25  30.00  64.81   97
  4  \w     -8.00  87.00   1.00   20.91    --   18.94  72.00 168.00   95
  5  \w     -4.00  80.00   1.00   20.91    --   18.94  77.00 -90.00   84
  6  \w    -59.00  -6.00   1.00   20.91    --  -19.25  19.00  30.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0393992000
_diffrn_orient_matrix_UB_12      0.0230558000
_diffrn_orient_matrix_UB_13      0.0086906000
_diffrn_orient_matrix_UB_21      -0.0497216000
_diffrn_orient_matrix_UB_22      -0.0323881000
_diffrn_orient_matrix_UB_23      -0.0354677000
_diffrn_orient_matrix_UB_31      -0.0126067000
_diffrn_orient_matrix_UB_32      -0.0304535000
_diffrn_orient_matrix_UB_33      0.0258811000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_av_unetI/netI     0.1352
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20571
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.85
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.792
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60095
_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_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1277
_refine_diff_density_max         2.572
_refine_diff_density_min         -1.842
_refine_diff_density_rms         0.266
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         10024
_refine_ls_number_restraints     278
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1102
_refine_ls_R_factor_gt           0.0777
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1097P)^2^+20.4482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2090
_refine_ls_wR_factor_ref         0.2426
_reflns_number_gt                6764
_reflns_number_total             10024
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            am0c09940_si_002.cif
_cod_data_source_block           p170319e27
_cod_depositor_comments          'Adding full bibliography for 4517961.cif.'
_cod_original_cell_volume        2850.9(3)
_cod_original_formula_sum        'C84 H64 Eu5 N2 O47.50'
_cod_database_code               4517961
_chemical_oxdiff_formula         'C O Eu'
_chemical_oxdiff_usercomment     678-15
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O3AA) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(C33) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O2AA) \\sim Ueq: with sigma of 0.0005 and sigma for terminal atoms of
0.0005
Uanis(C1) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.05
Uanis(O2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
4. Others
 Fixed Sof: O3AA(0.75)
5.a Secondary CH2 refined with riding coordinates:
 C8AA(H8AA,H8AB), C25(H25A,H25B), C27(H27A,H27B), C43(H43A,H43B), C68(H68A,
 H68B), C79(H79A,H79B)
5.b Aromatic/amide H refined with riding coordinates:
 C48(H48), C5AA(H5AA), C9AA(H9AA), C29(H29), C36(H36), C6AA(H6AA), C62(H62),
 C69(H69), C74(H74), C81(H81), C3AA(H3AA)
5.c Idealised Me refined as rotating group:
 C106(H10A,H10B,H10C), C108(H10D,H10E,H10F), C0AA(H0AA,H0AB,H0AC)
;
_olex2_date_sample_data_collection 2017-03-19
_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 1.903
_oxdiff_exptl_absorpt_empirical_full_min 0.596