Soft crystalline properties of 2D frameworks constructed from lithium ions and dinitriles.
Nishiguchi, Taichi; Kageyama, Kotoha; Kurihara, Takuya; Shimanaka, Nanae; Tokuda, Shun; Tsuda, Shuto; Ma, Nattapol; Horike, Satoshi; Chemical science 17 (2026) 3669–3674; doi:10.1039/d5sc06222e

data_1576601
_publ_section_title
;
 Soft crystalline properties of 2D frameworks constructed from lithium
 ions and dinitriles.
;
_journal_issue                   7
_journal_name_full               'Chemical science'
_journal_page_first              3669
_journal_page_last               3674
_journal_paper_doi               10.1039/d5sc06222e
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         'F2 N O4 S2, C9 H10 Li N4'
_chemical_formula_sum            'C9 H10 F2 Li N5 O4 S2'
_chemical_formula_weight         361.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-06-10 deposited with the CCDC.	2025-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.1756(4)
_cell_length_b                   15.2002(13)
_cell_length_c                   20.2029(15)
_cell_measurement_reflns_used    3805
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.5910
_cell_measurement_theta_min      2.8170
_cell_volume                     1589.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.933
_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    -62.00 -36.00   0.50    1.19    --    4.00  45.00 150.00   52
  2  \w    -58.00 -32.00   0.50    1.19    --  -16.60  45.00 150.00   52
  3  \w      1.00  34.00   0.50    1.19    --  -16.60  45.00 150.00   66
  4  \w     36.00  62.00   0.50    1.19    --  -16.60  45.00 150.00   52
  5  \w     38.00  63.00   0.50    1.19    --  -16.60  45.00   0.00   50
  6  \w   -106.00  71.00   0.50    1.19    --  -16.60  45.00 120.00  354
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0064414000
_diffrn_orient_matrix_UB_12      -0.0456870000
_diffrn_orient_matrix_UB_13      -0.0068948000
_diffrn_orient_matrix_UB_21      0.0384575000
_diffrn_orient_matrix_UB_22      0.0094762000
_diffrn_orient_matrix_UB_23      -0.0329289000
_diffrn_orient_matrix_UB_31      0.1315221000
_diffrn_orient_matrix_UB_32      -0.0006575000
_diffrn_orient_matrix_UB_33      0.0099185000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            11720
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.203
_diffrn_reflns_theta_min         2.680
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.379
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16313
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
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    1.510
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2473
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0630
_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^)+(0.0931P)^2^+0.3026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1841
_refine_ls_wR_factor_ref         0.2039
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1625
_reflns_number_total             2473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc06222e2.cif
_cod_data_source_block           230831_8_kageyama_fsg_1_4_3_0degc_auto
_cod_depositor_comments
'Adding full bibliography for 1576599--1576601.cif.'
_cod_database_code               1576601
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Li C11 H10 N3 O4 S2 F6'
_chemical_oxdiff_usercomment     0degC
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Shared sites
{S1, S1A}
3. Restrained distances
 N2-C4 = N2-C4A
 1.136 with sigma of 0.02
 C4-C5 = C4A-C5A
 1.47 with sigma of 0.02
 F1-S1 = F1A-S1A
 1.527 with sigma of 0.02
 O2-S1 = O1-S1 = O2A-S1A = O1A-S1A
 1.428 with sigma of 0.02
 N2-C5 \\sim N2-C5A
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(N3) \\sim Ueq, Uanis(S1) \\sim Ueq, Uanis(S1A) \\sim Ueq, Uanis(O2) \\sim
Ueq, Uanis(F1A) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(O2A) \\sim Ueq: with
sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(S1) = Uanis(S1A)
5. Rigid body (RIGU) restrains
 N3, S1, O2, F1, S1A, F1A, O2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C4A)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=1-FVAR(1)
 Sof(C4)=Sof(C5)=Sof(H5A)=Sof(H5B)=FVAR(1)
 Sof(O1A)=Sof(S1A)=Sof(F1A)=Sof(O2A)=1-FVAR(2)
 Sof(S1)=Sof(O1)=Sof(O2)=Sof(F1)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C5A(H5AA,H5AB)
;
_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 4.394
_oxdiff_exptl_absorpt_empirical_full_min 0.586