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_7251438
_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         'C18.325 H16.091 Mn N3.442 O9.442, 1.5[H2O]'
_chemical_formula_sum            'C18.33 H19.09 Mn N3.44 O10.94'
_chemical_formula_weight         517.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 99.72(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.934(6)
_cell_length_b                   4.7500(9)
_cell_length_c                   29.072(6)
_cell_measurement_reflns_used    18180
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      31.712
_cell_measurement_theta_min      1.294
_cell_volume                     4346.5(15)
_computing_cell_refinement       'XDS (Kabsch, 1999)'
_computing_data_collection       'BluICE (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1999)'
_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_temperature      100.15
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.829
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.0964
_diffrn_reflns_av_unetI/netI     0.1105
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.829
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            18180
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.829
_diffrn_reflns_theta_full        25.244
_diffrn_reflns_theta_max         31.712
_diffrn_reflns_theta_min         1.294
_diffrn_source                   'MX1 Australian Synchtrotron'
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_T_max  'Value not supplied by XDS'
_exptl_absorpt_correction_T_min  'Value not supplied by XDS'
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       needle
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.029
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         6091
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1431
_refine_ls_R_factor_gt           0.0980
_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^)+(0.1944P)^2^+2.0942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2783
_refine_ls_wR_factor_ref         0.3254
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3590
_reflns_number_total             6091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00993f2.cif
_cod_data_source_block           2Mn
_cod_original_cell_volume        4346.6(15)
_cod_database_code               7251438
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.936
_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. Uiso/Uaniso restraints and constraints
Uanis(C20A) \\sim Ueq, Uanis(N4A) \\sim Ueq, Uanis(N4B) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.2
Uanis(C20B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
Uanis(C18A) \\sim Ueq, Uanis(C18B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.2
3. Others
 Sof(Mn1)=Sof(O9)=Sof(O10B)=Sof(N3)=Sof(N4B)=Sof(C15)=Sof(H15)=Sof(C16)=
 Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18B)=
 Sof(H18B)=Sof(C19B)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C20B)=Sof(H20D)=
 Sof(H20E)=Sof(H20F)=1-FVAR(1)
 Sof(Mn2)=Sof(O10A)=Sof(N4A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(H19B)=
 Sof(H19C)=Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C13(H13A,H13B)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C15(H15), C18A(H18A), C18B(H18B)
4.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19A(H19A,H19B,H19C), C19B(H19D,
 H19E,H19F), C20A(H20A,H20B,H20C), C20B(H20D,H20E,H20F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2805
_shelx_fab_checksum              70634
_olex2_submission_special_instructions 'No special instructions were received'