A new type of lanthanide-sodium metalloring organic framework featuring high proton conduction in a wide temperature range and detection of Fe<sup>3+</sup> ions.
Liu, Lizhen; Zhu, Gaoyong; Yang, Kang; Chen, Yaozong; Hong, Yuan; Bo, Yiyang; Wu, Susu; Peng, Xiangfang; Yao, Zizhu; Dalton transactions (Cambridge, England : 2003) 54 (2024) 259–266; doi:10.1039/d4dt02479f

data_7717408
_publ_section_title
;
 A new type of lanthanide-sodium metalloring organic framework featuring
 high proton conduction in a wide temperature range and detection of
 Fe<sup>3+</sup> ions.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              259
_journal_page_last               266
_journal_paper_doi               10.1039/d4dt02479f
_journal_volume                  54
_journal_year                    2024
_chemical_formula_moiety
'C32 H2 Eu2 Na1.5 O30 S4, O, 1.25[C2H8N], 4.25[H3O], 6[H2O], 0.5[CH3OH], 1[C4H9NO]'
_chemical_formula_sum            'C32 H14 Eu2 Na1.5 O31 S4'
_chemical_formula_weight         1361.08
_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     dual
_audit_creation_date             2024-10-30
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-10-30 deposited with the CCDC.	2024-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.7240(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.1324(3)
_cell_length_b                   27.9543(5)
_cell_length_c                   22.9415(4)
_cell_measurement_reflns_used    17466
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.6320
_cell_measurement_theta_min      4.3540
_cell_volume                     15336.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5148
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.999
_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   -115.00 -16.00   1.00    7.50    --  -40.70 -38.00-120.00   99
  2  \w    -65.00  34.00   1.00    7.50    --  -40.70  38.00  90.00   99
  3  \w      1.00  82.00   1.00    7.50    --   40.70 -99.00-150.00   81
  4  \w      1.00  82.00   1.00    7.50    --   40.70 -99.00  60.00   81
  5  \w     21.00 109.00   1.00   17.50    --  103.24 -94.00  30.00   88
  6  \w     77.00 176.00   1.00   17.50    --  103.24  45.00-120.00   99
  7  \w     74.00 176.00   1.00   17.50    --  103.24  61.00-120.00  102
  8  \w     77.00 177.00   1.00   17.50    --  103.24  30.00 150.00  100
  9  \w     32.00 127.00   1.00   17.50    --  103.24 -61.00  90.00   95
 10  \w     84.00 177.00   1.00   17.50    --  103.24  77.00-180.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0052592000
_diffrn_orient_matrix_UB_12      -0.0474144000
_diffrn_orient_matrix_UB_13      0.0329918000
_diffrn_orient_matrix_UB_21      -0.0629903000
_diffrn_orient_matrix_UB_22      0.0092958000
_diffrn_orient_matrix_UB_23      -0.0004082000
_diffrn_orient_matrix_UB_31      -0.0124048000
_diffrn_orient_matrix_UB_32      -0.0264661000
_diffrn_orient_matrix_UB_33      -0.0592241000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            40468
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         3.697
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.245
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_description       block
_exptl_crystal_F_000             5284
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.753
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         13532
_refine_ls_number_restraints     325
_refine_ls_restrained_S_all      2.012
_refine_ls_R_factor_all          0.1016
_refine_ls_R_factor_gt           0.0859
_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^)+(0.1488P)^2^+168.3729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2376
_refine_ls_wR_factor_ref         0.2542
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10687
_reflns_number_total             13532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02479f2.cif
_cod_data_source_block           FUT-2-Eu
_cod_depositor_comments
'Adding full bibliography for 7717408--7717409.cif.'
_cod_original_formula_sum        'C32 H14 Eu2 Na1.50 O31 S4'
_cod_database_code               7717408
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C1 H1 O1 N1 S1 Eu1'
_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
 O18-O30
 2.4 with sigma of 0.02
 S3-O30
 1.45 with sigma of 0.02
 S3-O18 = S3-O17
 1.45 with sigma of 0.01
 S2-O5 = S2-O6 = S2-O32
 1.43 with sigma of 0.02
 S3-O30 = S3-O30A = S3-O17 = S3-O17A = S3-O18 = S3-O18A
 1.43 with sigma of 0.02
 O30A-O17A
 2.4 with sigma of 0.02
 O30-O18
 2.4 with sigma of 0.02
 O17A-O18A
 2.4 with sigma of 0.02
 O18-O17
 2.4 with sigma of 0.02
 O18A-O30A
 2.4 with sigma of 0.02
 O17-O30
 2.4 with sigma of 0.02
 S3-O18 \\sim S3-O18A
 with sigma of 0.02
 S3-O17 \\sim S3-O17A
 with sigma of 0.02
 S3-O30 \\sim S3-O30A
 with sigma of 0.02
3. Rigid bond restraints
 S3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C12, O12, O31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C5, C6, C7, C3, C2, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O18 \\sim O30 \\sim O17 \\sim S3 \\sim C31 \\sim C30 \\sim C28 \\sim C27 \\sim
C26 \\sim C32: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
O18 \\sim S3 \\sim O30 \\sim O17 \\sim C31 \\sim C30 \\sim C28 \\sim C27 \\sim
C26 \\sim C32: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 1.7A
S3: within 1.7A with sigma of 0.001 and sigma for terminal atoms of 0.002
within 1.7A
C12 \\sim O12 \\sim O31 \\sim C11 \\sim C13 \\sim C14 \\sim C15 \\sim C9 \\sim
C10 \\sim S1 \\sim O10 \\sim O9 \\sim O8 \\sim O14 \\sim O13: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
O12 \\sim C12 \\sim O31: within 1.7A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 1.7A
O2 \\sim C1 \\sim O1: within 1.7A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 1.7A
C4 \\sim C2 \\sim C3 \\sim C7 \\sim C6 \\sim C5: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 1.7A
C5 \\sim C6 \\sim C7 \\sim C3 \\sim C2 \\sim C4: within 1.7A with sigma of
0.001 and sigma for terminal atoms of 0.002 within 1.7A
O26 \\sim O24 \\sim S4 \\sim O25: within 1.7A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 1.7A
Uanis(O18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O27) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O30) \\sim Ueq, Uanis(O17) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Eu2) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(C16) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O32) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(S3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O30A) \\sim Ueq, Uanis(O17A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O18A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: O17(0.75) O30(0.75) O18(0.75) O18A(0.25) O30A(0.25) O17A(0.25)
 O11(0.5)
6.a Rotating group:
 O10W(H10A,H10B)
6.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C13(H13), C19(H19), C3(H3), C15(H15), C27(H27), C24(H24), C22(H22),
 C30(H30), C32(H32), C6(H6), C4(H4)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 0.8
_shelx_res_checksum              3191
_shelx_hkl_checksum              67497
_shelx_fab_checksum              58322
_olex2_date_sample_data_collection 2021-07-12
_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 4.072
_oxdiff_exptl_absorpt_empirical_full_min 0.522