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_7717409
_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 H14 Na1.5 O30 S4 Sm2, 0.5(H2 O)'
_chemical_formula_sum            'C32 H15 Na1.5 O30.5 S4 Sm2'
_chemical_formula_weight         1350.86
_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                 98.693(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.1627(12)
_cell_length_b                   28.0873(12)
_cell_length_c                   22.9131(7)
_cell_measurement_reflns_used    12707
_cell_measurement_temperature    299.58(10)
_cell_measurement_theta_max      74.1240
_cell_measurement_theta_min      2.3760
_cell_volume                     15371.7(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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      air
_diffrn_ambient_temperature      299.58(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.985
_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    -65.00 -36.00   0.50    0.15    -- -104.50  61.00 -30.00   58
  2  \w    -21.00  30.00   0.50    0.05    --  -45.83  19.00  30.00  102
  3  \w    -21.00  29.00   0.50    0.05    --  -45.83  19.00 -30.00  100
  4  \w     37.00  87.00   0.50    0.15    --  108.75 -95.00-180.00  100
  5  \w     37.00 102.00   0.50    0.15    --  108.75 -95.00 -90.00  130
  6  \w     63.00 105.00   0.50    0.15    --  108.75 -94.00-152.00   84
  7  \w     53.00  79.00   0.50    0.15    --  108.75-125.00 -30.00   52
  8  \w     40.00  68.00   0.50    0.15    --  108.75 -95.00  30.00   56
  9  \w     80.00 105.00   0.50    0.15    --  108.75 -95.00   0.00   50
 10  \w    -21.00  78.00   0.50    0.05    --   45.83 -94.00-152.00  198
 11  \w     53.00  78.00   0.50    0.15    --  108.75 -81.00-129.03   50
 12  \w     82.00 108.00   0.50    0.15    --  108.75 -81.00-129.03   52
 13  \w     82.00 108.00   0.50    0.15    --  108.75 -81.00-147.90   52
 14  \w     36.00  65.00   0.50    0.15    --  108.75 -81.00-147.90   58
 15  \w     66.00 109.00   0.50    0.15    --  108.75 -77.00-120.00   86
 16  \w     38.00  67.00   0.50    0.15    --  108.75 -61.00 -90.00   58
 17  \w     36.00  74.00   0.50    0.15    --  108.75 -61.00 -60.00   76
 18  \w     37.00  62.00   0.50    0.15    --  108.75 -61.00-120.00   50
 19  \w     38.00  63.00   0.50    0.15    --  108.75 -61.00-150.00   50
 20  \w     45.00  87.00   0.50    0.15    --  108.75 -77.00   0.00   84
 21  \w     43.00  73.00   0.50    0.15    --  108.75 -61.00   0.00   60
 22  \w     37.00  63.00   0.50    0.15    --  108.75 -61.00  30.00   52
 23  \w     37.00  64.00   0.50    0.15    --  108.75 -59.00 102.61   54
 24  \w     43.00  68.00   0.50    0.15    --  108.75 -69.00 148.66   50
 25  \w    -29.00  28.00   0.50    0.05    --   45.83 -19.00  90.00  114
 26  \w     56.00  94.00   0.50    0.15    --  108.75  -1.00-148.90   76
 27  \w    116.00 174.00   0.50    0.15    --  108.75  -1.00-148.90  116
 28  \w    142.00 169.00   0.50    0.15    --  108.75  30.00-120.00   54
 29  \w    142.00 176.00   0.50    0.15    --  108.75  60.00-130.81   68
 30  \w    140.00 165.00   0.50    0.15    --  108.75  77.00-120.00   50
 31  \w     85.00 136.00   0.50    0.15    --  108.75  77.00-120.00  102
 32  \w    101.00 127.00   0.50    0.15    --  108.75  60.00-130.81   52
 33  \w    103.00 129.00   0.50    0.15    --  108.75  30.00 -60.00   52
 34  \w     94.00 145.00   0.50    0.15    --  108.75  45.00   0.00  102
 35  \w    126.00 177.00   0.50    0.15    --  108.75  45.00  30.00  102
 36  \w    120.00 176.00   0.50    0.15    --  108.75  61.00  60.00  112
 37  \w    148.00 175.00   0.50    0.15    --  108.75  61.00 120.00   54
 38  \w     94.00 138.00   0.50    0.15    --  108.75  30.00-120.00   88
 39  \w    134.00 159.00   0.50    0.15    --  108.75  94.00 -41.00   50
 40  \w     -7.00  21.00   0.50    0.05    --  -45.83  94.00 -41.00   56
 41  \w     81.00 113.00   0.50    0.15    --  108.75 125.00  90.00   64
 42  \w    138.00 168.00   0.50    0.15    --  108.75 125.00  90.00   60
 43  \w    -69.00 -22.00   0.50    0.05    --  -45.83  94.00 -41.00   94
 44  \w    -92.00 -67.00   0.50    0.15    -- -104.50  94.00 -41.00   50
 45  \w   -115.00 -90.00   0.50    0.15    -- -104.50 -53.00 -94.52   50
 46  \w   -127.00 -89.00   0.50    0.15    -- -104.50 -94.00-152.00   76
 47  \w   -160.00-134.00   0.50    0.15    -- -104.50 -53.00 -94.52   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0619521000
_diffrn_orient_matrix_UB_12      0.0048512000
_diffrn_orient_matrix_UB_13      -0.0077808000
_diffrn_orient_matrix_UB_21      -0.0113103000
_diffrn_orient_matrix_UB_22      0.0509100000
_diffrn_orient_matrix_UB_23      -0.0239522000
_diffrn_orient_matrix_UB_31      0.0138018000
_diffrn_orient_matrix_UB_32      0.0198284000
_diffrn_orient_matrix_UB_33      0.0632302000
_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  0.1375
_diffrn_reflns_av_unetI/netI     0.0864
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            79131
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.073
_diffrn_reflns_theta_min         2.428
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.998
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_description       needle
_exptl_crystal_F_000             5244
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.686
_refine_diff_density_min         -2.143
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         13708
_refine_ls_number_restraints     372
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0863
_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^)+(0.1716P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2382
_refine_ls_wR_factor_ref         0.2496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10772
_reflns_number_total             13708
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02479f2.cif
_cod_data_source_block           FUT-2-Sm
_cod_depositor_comments
'Adding full bibliography for 7717408--7717409.cif.'
_cod_original_formula_sum        'C32 H15 Na1.50 O30.50 S4 Sm2'
_cod_database_code               7717409
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
2. Restrained distances
 O18-O16
 2.327 with sigma of 0.02
 S2-O10 = S2-O30
 1.43 with sigma of 0.02
 S2-O30
 1.45 with sigma of 0.01
 S2-O10
 1.45 with sigma of 0.01
 S3-O18
 1.42 with sigma of 0.02
 S3-O16
 1.4 with sigma of 0.02
 O16-O18
 2.373 with sigma of 0.02
 S3-O17
 1.42 with sigma of 0.02
 O17-O18
 2.346 with sigma of 0.02
 O16-O17
 2.253 with sigma of 0.02
 O18-O17
 2.353 with sigma of 0.02
 O1W-O9
 2.8 with sigma of 0.02
 C8-C6
 1.45 with sigma of 0.01
 S4-O24
 1.42 with sigma of 0.01
 S3-O18 = S3-O17 = S3-O16
 1.42 with sigma of 0.02
 S3-O17 = S3-O18 = S3-O16
 1.45 with sigma of 0.01
 S3-O16 = S3-O17 = S3-O18
 1.47 with sigma of 0.01
 S2-C28
 1.8 with sigma of 0.02
 O30-O11
 2.35 with sigma of 0.02
 O30-O10
 2.35 with sigma of 0.02
 O10-O11
 2.35 with sigma of 0.02
 O17A-O16A
 2.4 with sigma of 0.02
 S3-O16A = S3-O18A = S3-O17A
 1.43 with sigma of 0.02
 O16A-O18A
 2.4 with sigma of 0.02
 O18A-O17A
 2.4 with sigma of 0.02
 S2-O30A = S2-O11A = S2-O10A
 1.43 with sigma of 0.02
 O10A-O30A
 2.4 with sigma of 0.02
 O10A-O11A
 2.4 with sigma of 0.02
 O30A-O11A
 2.4 with sigma of 0.02
 C32-C30
 1.5 with sigma of 0.01
 S3-O16 \\sim S3-O16A
 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
 S2-O30 \\sim S2-O30A
 with sigma of 0.02
 S2-O10 \\sim S2-O10A
 with sigma of 0.02
 S2-O11 \\sim S2-O11A
 with sigma of 0.02
3. Rigid bond restraints
 S2, C28, C27, C26, C31, C30, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O16, S3, O18, O17, C12, C11, C13, C14, C15, C10, C9, O21, O22, O19, C16, O20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
S2 \\sim C28 \\sim C27 \\sim C26 \\sim C31 \\sim C30 \\sim C29: within 1.7A
with sigma of 0.0001 and sigma for terminal atoms of 0.0002 within 1.7A
S2: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
1.7A
O16 \\sim S3 \\sim O18 \\sim O17 \\sim C12 \\sim C11 \\sim C10 \\sim C15 \\sim
C14 \\sim C13 \\sim C16 \\sim O20 \\sim O19 \\sim O21 \\sim C9 \\sim O22:
within 1.7A with sigma of 0.0001 and sigma for terminal atoms of 0.0002 within
1.7A
C28 \\sim C29 \\sim C30 \\sim C31 \\sim C26 \\sim C27: within 1.7A with sigma
of 0.001 and sigma for terminal atoms of 0.002 within 1.7A
O30 \\sim O11 \\sim O10 \\sim S2 \\sim C28 \\sim C29 \\sim C27 \\sim C26 \\sim
C30 \\sim C31: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
O16A \\sim O16 \\sim O18A \\sim O18 \\sim O17A \\sim O17: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
O11A \\sim O30 \\sim O30A \\sim O10 \\sim O10A \\sim O11: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O30) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O25) \\sim Ueq, Uanis(O23) \\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(O16A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O30A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: O18(0.75) O16(0.75) O17(0.75) O9(0.5) H9A(0.5) H9B(0.5) O10(0.5)
 O30(0.5) O11(0.5) O18A(0.25) O16A(0.25) O17A(0.25) O30A(0.5) O10A(0.5)
 O11A(0.5)
6.a Riding coordinates:
 O1W(H1WA,H1WB), O9(H9A,H9B)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C15(H15), C31(H31), C19(H19), C7(H7), C24(H24), C22(H22),
 C13(H13), C29(H29), C11(H11), C27(H27)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              37100
_shelx_hkl_checksum              20432
_shelx_fab_checksum              34529
_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 2.222
_oxdiff_exptl_absorpt_empirical_full_min 0.476