Conformational preferences of diimide-based dicarboxylate species and their coordination polymers
Cao, Winnie; Glascott, Bianca K.; Izgorodina, Ekaterina I.; Turner, David R.; CrystEngComm 28 (2026) 736–747; doi:10.1039/D5CE00993F

data_7251441
_publ_section_title
;
 Conformational preferences of diimide-based dicarboxylate species and
 their coordination polymers
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              736
_journal_page_last               747
_journal_paper_doi               10.1039/D5CE00993F
_journal_volume                  28
_journal_year                    2026
_chemical_formula_moiety         'C18 H16 N2 O8'
_chemical_formula_sum            'C18 H16 N2 O8'
_chemical_formula_weight         388.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-07-09
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-09-08 deposited with the CCDC.	2025-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                85.726(3)
_cell_angle_beta                 80.660(3)
_cell_angle_gamma                81.607(3)
_cell_formula_units_Z            1
_cell_length_a                   5.7316(2)
_cell_length_b                   6.1988(2)
_cell_length_c                   12.4730(5)
_cell_measurement_reflns_used    2667
_cell_measurement_temperature    122.99(10)
_cell_measurement_theta_max      76.4360
_cell_measurement_theta_min      3.5830
_cell_volume                     432.01(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.944
_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   -103.00 -51.00   0.50    0.05    --  -47.45-155.00  16.00  104
  2  \w   -119.00 -74.00   0.50    0.05    --  -47.45-125.00 -30.00   90
  3  \w   -142.00 -98.00   0.50    0.05    --  -86.25-155.00  16.00   88
  4  \w   -137.00 -70.00   0.50    0.05    --  -86.25-125.00 120.00  134
  5  \w   -116.00 -80.00   0.50    0.05    --  -47.45-120.00 172.00   72
  6  \w   -117.00 -75.00   0.50    0.05    --  -86.25-120.00 172.00   84
  7  \w     36.00  61.00   0.50    0.05    --   47.45-120.00 172.00   50
  8  \w     35.00  83.00   0.50    0.05    --  107.75-120.00 172.00   96
  9  \w     88.00 113.00   0.50    0.05    --  107.75-120.00 172.00   50
 10  \w     51.00  82.00   0.50    0.05    --  107.75-125.00 120.00   62
 11  \w     92.00 117.00   0.50    0.05    --  107.75-155.00  16.00   50
 12  \w     76.00 106.00   0.50    0.05    --   47.45-155.00  16.00   60
 13  \w     39.00  69.00   0.50    0.05    --  107.75 -99.00   0.00   60
 14  \w     61.00  87.00   0.50    0.05    --  107.75 -38.00 -60.00   52
 15  \w     36.00 108.00   0.50    0.05    --  107.75 -99.00-150.00  144
 16  \w     36.00 116.00   0.50    0.05    --  107.75-125.00 -30.00  160
 17  \w     39.00  78.00   0.50    0.05    --  107.75 -38.00 120.00   78
 18  \w     87.00 116.00   0.50    0.05    --  107.75 -38.00 120.00   58
 19  \w     96.00 175.00   0.50    0.05    --  107.75  38.00 -30.00  158
 20  \w    146.00 172.00   0.50    0.05    --  107.75  38.00-120.00   52
 21  \w    112.00 137.00   0.50    0.05    --  107.75 120.00-102.00   50
 22  \w     98.00 174.00   0.50    0.05    --  107.75 125.00-180.00  152
 23  \w    101.00 128.00   0.50    0.05    --  107.75  38.00-120.00   54
 24  \w     78.00 103.00   0.50    0.05    --   47.45 155.00  53.00   50
 25  \w     95.00 120.00   0.50    0.05    --  107.75 155.00  53.00   50
 26  \w    -25.00  22.00   0.50    0.05    --   47.45 -38.00  60.00   94
 27  \w     28.00  56.00   0.50    0.05    --   47.45 -38.00  60.00   56
 28  \w     -1.00  58.00   0.50    0.05    --   47.45 -99.00   0.00  118
 29  \w     41.00 106.00   0.50    0.05    --  107.75 -99.00  30.00  130
 30  \w    -71.00 -46.00   0.50    0.05    --  -47.45 120.00-102.00   50
 31  \w    -57.00 -32.00   0.50    0.05    --  -86.25 120.00-102.00   50
 32  \w    -88.00 -62.00   0.50    0.05    --  -47.45 155.00  53.00   52
 33  \w   -162.00 -99.00   0.50    0.05    --  -86.25 -19.00-150.00  126
 34  \w   -145.00-112.00   0.50    0.05    --  -86.25 -57.00-180.00   66
;
_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      -0.1570272000
_diffrn_orient_matrix_UB_12      0.0961196000
_diffrn_orient_matrix_UB_13      0.1021679000
_diffrn_orient_matrix_UB_21      0.1081908000
_diffrn_orient_matrix_UB_22      -0.1907481000
_diffrn_orient_matrix_UB_23      0.0709254000
_diffrn_orient_matrix_UB_31      0.1980769000
_diffrn_orient_matrix_UB_32      0.1328827000
_diffrn_orient_matrix_UB_33      0.0155512000
_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  0.0333
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4416
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.979
_diffrn_reflns_theta_min         3.596
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.020
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43041
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       plate
_exptl_crystal_F_000             202
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         1726
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0764P)^2^+0.3889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1599
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1559
_reflns_number_total             1726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00993f2.cif
_cod_data_source_block           H2ibaPmDI
_cod_database_code               7251441
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C10O4N2H20
_cell_oxdiff_angle_alpha         85.726(3)
_cell_oxdiff_angle_beta          80.660(3)
_cell_oxdiff_angle_gamma         81.607(3)
_cell_oxdiff_length_a            5.7316(2)
_cell_oxdiff_length_b            6.1988(2)
_cell_oxdiff_length_c            12.4730(5)
_cell_oxdiff_measurement_reflns_used 2667
_cell_oxdiff_volume              432.01(3)
_diffrn_oxdiff_ac3_digest_frames
;
01532063d6c56c8e737d0b12cc2c6abb7c00089f576
;
_diffrn_oxdiff_ac3_digest_hkl
;
01c22f9992bfe8b11cfca8498dbf3bce4130da
;
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-H1
 0.84 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C9(H9)
3.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              79711
_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 1.666
_oxdiff_exptl_absorpt_empirical_full_min 0.574