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_7251445
_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 Co N4 O10'
_chemical_formula_sum            'C20 H20 Co N4 O10'
_chemical_formula_weight         535.33
_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   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                84.244(4)
_cell_angle_beta                 71.817(4)
_cell_angle_gamma                63.400(6)
_cell_formula_units_Z            2
_cell_length_a                   9.6362(5)
_cell_length_b                   10.1021(7)
_cell_length_c                   13.5166(6)
_cell_measurement_reflns_used    7451
_cell_measurement_temperature    123.0(2)
_cell_measurement_theta_max      75.4100
_cell_measurement_theta_min      4.7950
_cell_volume                     1116.56(13)
_computing_cell_refinement       'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 40.84a 64-bit (release 31-07-2020))'
_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      123.0(2)
_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 0.960
_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     25.00 120.00   0.50    2.50    --   47.64  77.00   0.00  190
  2  \w    105.00 178.00   0.50   11.00    --  107.75 107.00 -88.00  146
  3  \w     95.00 178.00   0.50   11.00    --  107.75  45.00 -30.00  166
  4  \w     95.00 178.00   0.50   11.00    --  107.75 125.00  60.00  166
  5  \w     95.00 178.00   0.50   11.00    --  107.75 125.00 150.00  166
  6  \w     36.00  76.00   0.50   11.00    --  107.75 -45.00  60.00   80
  7  \w     35.00 106.00   0.50   11.00    --  107.75 -94.00   0.00  142
  8  \w     36.00  76.00   0.50   11.00    --  107.75 -45.00-120.00   80
  9  \w     35.00 106.00   0.50   11.00    --  107.75 -94.00-150.00  142
 10  \w     36.00  76.00   0.50   11.00    --  107.75 -45.00 -30.00   80
 11  \w     33.00  66.00   0.50   11.00    --  107.75 -30.00 -30.00   66
 12  \w     35.00 124.00   0.50   11.00    --  107.75 -61.00   0.00  178
 13  \w     95.00 178.00   0.50   11.00    --  107.75  45.00-120.00  166
 14  \w     95.00 178.00   0.50   11.00    --  107.75  45.00-180.00  166
 15  \w     35.00 106.00   0.50   11.00    --  107.75 -94.00-180.00  142
 16  \w     36.00  76.00   0.50   11.00    --  107.75 -45.00-180.00   80
 17  \w     35.00 106.00   0.50   11.00    --  107.75 -94.00-120.00  142
 18  \w     36.00  76.00   0.50   11.00    --  107.75 -45.00-150.00   80
 19  \w     35.00 106.00   0.50   11.00    --  107.75-100.00-145.19  142
 20  \w     35.00 112.00   0.50   11.00    --  107.75-125.00-180.00  154
 21  \w     35.00 106.00   0.50   11.00    --  107.75 -94.00 -30.00  142
 22  \w     33.00  66.00   0.50   11.00    --  107.75 -30.00  30.00   66
 23  \w     33.00  66.00   0.50   11.00    --  107.75 -30.00   0.00   66
 24  \w     35.00 106.00   0.50   11.00    --  107.75 -94.00  60.00  142
 25  \w     36.00  76.00   0.50   11.00    --  107.75 -45.00 150.00   80
 26  \w     35.00 107.00   0.50   11.00    --  107.75-107.00 173.00  144
 27  \w     33.00  66.00   0.50   11.00    --  107.75 -30.00 120.00   66
 28  \w     35.00 106.00   0.50   11.00    --  107.75 -94.00  90.00  142
 29  \w     35.00 112.00   0.50   11.00    --  107.75-125.00 -30.00  154
 30  \w     20.00  86.00   0.50    2.50    --   47.64-107.00 173.00  132
 31  \w     33.00 120.00   0.50    2.50    --   47.64  57.00 120.00  174
 32  \w     25.00 120.00   0.50    2.50    --   47.64  77.00 -90.00  190
 33  \w     25.00 120.00   0.50    2.50    --   47.64  77.00-180.00  190
 34  \w    -61.00  25.00   0.50    2.50    --  -47.64  38.00-180.00  172
 35  \w    -61.00  25.00   0.50    2.50    --  -47.64  38.00 -60.00  172
 36  \w    -68.00 -11.00   0.50   11.00    --  -86.25  30.00  30.00  114
 37  \w    -81.00   1.00   0.50    2.50    --  -47.64 107.00 -88.00  164
 38  \w    -81.00 -13.00   0.50   11.00    --  -86.25 107.00 -88.00  136
 39  \w   -120.00 -34.00   0.50    2.50    --  -47.64 -38.00-150.00  172
 40  \w   -120.00 -33.00   0.50    2.50    --  -47.64 -57.00  30.00  174
 41  \w   -120.00 -66.00   0.50    2.50    --  -47.64 -77.00 120.00  108
 42  \w   -159.00 -83.00   0.50   11.00    --  -86.25-107.00 173.00  152
 43  \w   -161.00 -73.00   0.50   11.00    --  -86.25 -30.00  30.00  176
;
_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      -0.0347538000
_diffrn_orient_matrix_UB_12      0.1113111000
_diffrn_orient_matrix_UB_13      -0.0860636000
_diffrn_orient_matrix_UB_21      0.1579347000
_diffrn_orient_matrix_UB_22      -0.1078065000
_diffrn_orient_matrix_UB_23      -0.0787937000
_diffrn_orient_matrix_UB_31      -0.0947918000
_diffrn_orient_matrix_UB_32      -0.0716821000
_diffrn_orient_matrix_UB_33      -0.0284159000
_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  0.0892
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22192
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.632
_diffrn_reflns_theta_min         4.901
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.617
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72209
_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    1.592
_exptl_crystal_description       needle
_exptl_crystal_F_000             550
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.106
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         4614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0751
_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^)+(0.1611P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2171
_refine_ls_wR_factor_ref         0.2322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3213
_reflns_number_total             4614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00993f2.cif
_cod_data_source_block           1Co
_cod_original_cell_volume        1116.56(12)
_cod_database_code               7251445
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Co'
_cell_oxdiff_angle_alpha         84.244(4)
_cell_oxdiff_angle_beta          71.817(4)
_cell_oxdiff_angle_gamma         63.400(6)
_cell_oxdiff_length_a            9.6362(4)
_cell_oxdiff_length_b            10.1021(7)
_cell_oxdiff_length_c            13.5166(6)
_cell_oxdiff_measurement_reflns_used 7451
_cell_oxdiff_volume              1116.56(10)
_diffrn_oxdiff_digest_hkl
;
0130f9d311e804ae5c4d62f6e26bce66b40f38
;
_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.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C15(H15), C18(H18)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              56219
_shelx_fab_checksum              95223
_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 2.866
_oxdiff_exptl_absorpt_empirical_full_min 0.406