The ratiometric detection of the biomarker Ap5A for dry eye disease and physiological temperature using a rare trinuclear lanthanide metal-organic framework.
Xia, Tifeng; Wan, Yating; Yan, Xiayan; Hu, Li; Wu, Zhigang; Zhang, Jun; Dalton transactions (Cambridge, England : 2003) 50 (2021) 2792–2799; doi:10.1039/d0dt03647a

data_7706456
_publ_section_title
;
 The ratiometric detection of the biomarker Ap5A for dry eye disease and
 physiological temperature using a rare trinuclear lanthanide
 metal-organic framework.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2792
_journal_page_last               2799
_journal_paper_doi               10.1039/d0dt03647a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'0.5(C76 H46 Eu6 O36), 1(O), 0.96(C O), 0.33(H6 O3)'
_chemical_formula_sum            'C38.96 H25 Eu3 O20.96'
_chemical_formula_weight         1284.35
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc26fd02
_audit_creation_date             2021-01-14
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.08.17 svn.r3210 for OlexSys, GUI svn.r5083)
;
_audit_update_record
;
2021-01-18 deposited with the CCDC.	2021-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   10.5738(4)
_cell_length_b                   10.5738(4)
_cell_length_c                   24.7974(10)
_cell_measurement_reflns_used    7901
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.040
_cell_measurement_theta_min      2.224
_cell_volume                     2401.04(16)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0108
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19898
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        23.140
_diffrn_reflns_theta_max         23.140
_diffrn_reflns_theta_min         1.642
_exptl_absorpt_coefficient_mu    3.944
_exptl_absorpt_correction_T_max  0.437
_exptl_absorpt_correction_T_min  0.345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0648 before and 0.0340 after correction.
The Ratio of minimum to maximum transmission is 0.8506.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_description       block
_exptl_crystal_F_000             1231
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.285
_refine_diff_density_min         -1.621
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         1167
_refine_ls_number_restraints     193
_refine_ls_restrained_S_all      2.283
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0479P)^2^+15.6096P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1100
_reflns_number_total             1167
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03647a2.cif
_cod_data_source_block           EuNDC
_cod_depositor_comments          'Adding full bibliography for 7706456.cif.'
_cod_original_cell_volume        2401.0(2)
_cod_database_code               7706456
_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
 C7-O3
 1.3 with sigma of 0.02
 C7-O4
 1.3 with sigma of 0.02
 C8-O6
 1.25 with sigma of 0.001
 O5-H5
 0.85 with sigma of 0.001
 H3AA-O3A
 0.85 with sigma of 0.001
 O3A-H3AB
 0.85 with sigma of 0.001
 O3-C7 \\sim C7-O4
 with sigma of 0.02
 Eu1-H5_$3 \\sim H5_$3-Eu1_$4
 with sigma of 0.02
 Eu1_$4-H5_$3 \\sim H5_$3-Eu1_$3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O4 \\sim O3 \\sim C7 \\sim O3A \\sim O4A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(O4) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O2A) = Uanis(O2)
Uanis(C8) = Uanis(O6)
Uanis(C0AA) = Uanis(C2A)
Uanis(C6A) = Uanis(C1AA)
Uanis(C3) = Uanis(C3A)
Uanis(C4A) = Uanis(C4)
Uanis(C5) = Uanis(C5A)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C0AA)=Sof(C1AA)=Sof(H1AA)=1-FVAR(1)
 Sof(C2A)=Sof(C6A)=Sof(H6A)=FVAR(1)
 Fixed Sof: O2(0.5) O1A(0.5) O1(0.5) O3(0.33333) O3A(0.16667) H3AA(0.16667)
 H3AB(0.16667) O4(0.33333) C1A(0.5) C1(0.5) C3(0.5) H3(0.5) C4(0.5) C5(0.5)
 H5A(0.5) C7(0.33333) H7(0.33333) O7(0.16667) O2A(0.5) O6(0.16) C8(0.16)
 O4A(0.16667) H4AA(0.16667) H4AB(0.16667) H5(0.16666) C3A(0.5) H3A(0.5)
 C4A(0.5) C5A(0.5) H5AA(0.5)
6.a Rotating group:
 O3A(H3AA,H3AB), O4A(H4AA,H4AB)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5A), C6A(H6A), C7(H7), C1AA(H1AA), C3A(H3A), C5A(H5AA)
;
_shelx_res_checksum              31650
_shelx_hkl_checksum              5263
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'