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_7251447
_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         'C20 H20 Cd N4 O10'
_chemical_formula_sum            'C20 H20 Cd N4 O10'
_chemical_formula_weight         588.80
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-10
_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                91.128(3)
_cell_angle_beta                 92.195(2)
_cell_angle_gamma                94.386(3)
_cell_formula_units_Z            1
_cell_length_a                   4.97300(10)
_cell_length_b                   9.0826(4)
_cell_length_c                   12.8166(4)
_cell_measurement_reflns_used    16090
_cell_measurement_temperature    123.00(11)
_cell_measurement_theta_max      29.9070
_cell_measurement_theta_min      2.7280
_cell_volume                     576.63(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 39.46 (release 15-03-2018))'
_computing_data_reduction        'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_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    -18.00  64.00   0.50    1.38    --   -8.50  38.00   0.00  164
  2  \w     -3.00  80.00   0.50    1.38    --    7.57  38.00-120.00  166
  3  \w    -14.00  80.00   0.50    1.38    --    7.57  77.00 120.00  188
  4  \w    -18.00  64.00   0.50    1.38    --   -8.50  38.00  90.00  164
  5  \w    -26.00  40.00   0.50    1.38    --    7.57 -99.00 -60.00  132
  6  \w      4.00  50.00   0.50    1.38    --    7.57-117.00-109.00   92
  7  \w    -26.00  24.00   0.50    1.38    --   -8.50 -99.00-180.00  100
  8  \w    -64.00  19.00   0.50    1.38    --    7.57 -38.00-150.00  166
  9  \w    -18.00  64.00   0.50    1.38    --   -8.50  38.00-180.00  164
 10  \w    -48.00 -21.00   0.50    1.38    --   -8.50 111.00 -70.83   54
 11  \w    -48.00 -22.00   0.50    1.38    --   -8.50 112.00-128.75   52
 12  \w    -48.00 -22.00   0.50    1.38    --   -8.00 112.00-163.28   52
 13  \w    -81.00  50.00   0.50    1.38    --   -8.50   0.00-180.00  262
 14  \w    -64.00  19.00   0.50    1.38    --    7.57 -38.00   0.00  166
 15  \w    -26.00  24.00   0.50    1.38    --   -8.50 -99.00  60.00  100
 16  \w     28.00  79.00   0.50    1.38    --    7.57-163.00 101.00  102
 17  \w    -67.00  19.00   0.50    1.38    --    7.57 -19.00  90.00  172
 18  \w    -64.00  19.00   0.50    1.38    --    7.57 -38.00 150.00  166
 19  \w    -64.00  19.00   0.50    1.38    --    7.57 -38.00 120.00  166
 20  \w    -67.00  19.00   0.50    1.38    --    7.57 -19.00  30.00  172
 21  \w    -64.00  19.00   0.50    1.38    --    7.57 -38.00 -60.00  166
 22  \w    -83.00   3.00   0.50    1.38    --   -8.50 -19.00 -30.00  172
 23  \w    -81.00   3.00   0.50    1.38    --   -8.50 -38.00-120.00  168
 24  \w    -81.00  50.00   0.50    1.38    --   -8.50   0.00-150.00  262
 25  \w    -81.00  50.00   0.50    1.38    --   -8.50   0.00-120.00  262
 26  \w    -38.00  16.00   0.50    1.38    --   -8.50  93.00 159.50  108
 27  \w    -48.00 -21.00   0.50    1.38    --   -8.50 111.00 177.49   54
 28  \w    -81.00  50.00   0.50    1.38    --   -8.50   0.00  30.00  262
 29  \w    -81.00  -5.00   0.50    1.38    --   -8.50   0.00  60.00  152
;
_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      -0.0058555000
_diffrn_orient_matrix_UB_12      -0.0706004000
_diffrn_orient_matrix_UB_13      0.0228648000
_diffrn_orient_matrix_UB_21      -0.0317595000
_diffrn_orient_matrix_UB_22      -0.0336727000
_diffrn_orient_matrix_UB_23      -0.0498022000
_diffrn_orient_matrix_UB_31      0.1394740000
_diffrn_orient_matrix_UB_32      -0.0044154000
_diffrn_orient_matrix_UB_33      -0.0081101000
_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  0.1281
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34715
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.992
_diffrn_reflns_theta_max         24.992
_diffrn_reflns_theta_min         2.726
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.010
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.95a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_description       needle
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2019
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0236
_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^)+(0.0169P)^2^+0.6237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1988
_reflns_number_total             2019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00993f2.cif
_cod_data_source_block           1Cd
_cod_database_code               7251447
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H20 Cd1 O2 N1'
_cell_oxdiff_angle_alpha         91.128(3)
_cell_oxdiff_angle_beta          92.195(2)
_cell_oxdiff_angle_gamma         94.386(3)
_cell_oxdiff_length_a            4.97298(11)
_cell_oxdiff_length_b            9.0826(4)
_cell_oxdiff_length_c            12.8166(4)
_cell_oxdiff_measurement_reflns_used 16090
_cell_oxdiff_volume              576.63(3)
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.676
_diffrn_oxdiff_digest_hkl
;
0126a3416eb07255032b1a2d83b8605b972160
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C8A)=Sof(H8A)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=Sof(C10B)=Sof(H10D)=
 Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(C8B)=Sof(H8B)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(H10A)=
 Sof(H10B)=Sof(H10C)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8A(H8A), C8B(H8B)
3.c Idealised Me refined as rotating group:
 C9A(H9AA,H9AB,H9AC), C9B(H9BA,H9BB,H9BC), C10A(H10A,H10B,H10C), C10B(H10D,
 H10E,H10F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              60916
_shelx_fab_checksum              19281
_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 2.136
_oxdiff_exptl_absorpt_empirical_full_min 0.292