Anthraquinone substituents modulate ionic hydrogen-bonded organic frameworks to achieve high ionic conductivity for alkali metal ions
Chen, Xu-Yong; Fei, Guiqiang; Bai, Xiang-Tian; Qi, Simeng; Cao, Xiao-Jie; Gao, Yi-Da; Luo, Xin; Cao, Li-Hui; Chemical Communications 61 (2025) 6538–6541; doi:10.1039/D5CC00747J

data_7134364
_publ_section_title
;
 Anthraquinone substituents modulate ionic hydrogen-bonded organic
 frameworks to achieve high ionic conductivity for alkali metal ions
;
_journal_issue                   35
_journal_name_full               'Chemical Communications'
_journal_page_first              6538
_journal_page_last               6541
_journal_paper_doi               10.1039/D5CC00747J
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C14 H6 O8 S2, 2(C H9 N6)'
_chemical_formula_sum            'C16 H24 N12 O8 S2'
_chemical_formula_weight         576.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-03-21
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-03-27 deposited with the CCDC.	2025-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.88320(10)
_cell_length_b                   14.6525(2)
_cell_length_c                   23.2897(4)
_cell_measurement_reflns_used    5105
_cell_measurement_temperature    212.99(10)
_cell_measurement_theta_max      76.1620
_cell_measurement_theta_min      6.0150
_cell_volume                     2348.91(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      212.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.941
_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  27.00   1.00    0.10    --   48.67 -19.00 150.00   49
  2  \w     39.00 110.00   1.00    0.10    --  106.65-122.00 161.00   71
  3  \w    -14.00  25.00   1.00    0.10    --   48.67 -17.00-127.00   39
  4  \w     60.00 103.00   1.00    0.10    --  106.65 -77.00-180.00   43
  5  \w    104.00 167.00   1.00    0.10    --  106.65 111.00 157.00   63
  6  \w     95.00 175.00   1.00    0.10    --  106.65  19.00  90.00   80
  7  \w   -160.00-101.00   1.00    0.10    --  -91.75 -17.00-127.00   59
  8  \w    -80.00 -54.00   1.00    0.10    --  -91.75 111.00 157.00   26
  9  \w    -27.00  26.00   1.00    0.10    --  -48.67  19.00 120.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0365804000
_diffrn_orient_matrix_UB_12      -0.0970665000
_diffrn_orient_matrix_UB_13      -0.0228393000
_diffrn_orient_matrix_UB_21      -0.0338122000
_diffrn_orient_matrix_UB_22      -0.0389073000
_diffrn_orient_matrix_UB_23      0.0606371000
_diffrn_orient_matrix_UB_31      -0.2183551000
_diffrn_orient_matrix_UB_32      -0.0103297000
_diffrn_orient_matrix_UB_33      -0.0132703000
_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  0.0373
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            7211
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.458
_diffrn_reflns_theta_min         6.040
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.708
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.0059(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         2327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0712P)^2^+0.8292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1127
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2122
_reflns_number_total             2327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00747j2.cif
_cod_data_source_block           cxy_5
_cod_depositor_comments
'Adding full bibliography for 7134363--7134364.cif.'
_cod_database_code               7134364
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         CHOS
_shelx_estimated_absorpt_t_max   0.687
_shelx_estimated_absorpt_t_min   0.613
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C6(H6), N1(H1), N5(H5), N3(H3)
;
_shelx_res_checksum              16656
_shelx_hkl_checksum              49804
_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 1.231
_oxdiff_exptl_absorpt_empirical_full_min 0.867