The crucial role of lattice water in directing supramolecular networks of deferiprone analogues: a combined X-ray and DFT study
García-Raso, Ángel; Rocha, Mariana; Terrón, Ángel; Fiol, Juan J.; López-Zafra, Adela; Rodríguez, Carlos A.; Vázquez-López, Ezequiel M.; Barceló-Oliver, Miquel; Frontera, Antonio; CrystEngComm 28 (2026) 951–961; doi:10.1039/D5CE01136A

data_7251500
_publ_section_title
;
 The crucial role of lattice water in directing supramolecular networks of
 deferiprone analogues: a combined X-ray and DFT study
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              951
_journal_page_last               961
_journal_paper_doi               10.1039/D5CE01136A
_journal_volume                  28
_journal_year                    2026
_chemical_formula_moiety         '0.667(Cl), H2 O, 0.667(C11 H14 N3 O2)'
_chemical_formula_sum            'C7.33 H11.33 Cl0.67 N2 O2.33'
_chemical_formula_weight         188.48
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-11-24 deposited with the CCDC.	2026-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.297(2)
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   51.723(3)
_cell_length_b                   7.3982(4)
_cell_length_c                   13.4262(8)
_cell_measurement_reflns_used    9672
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.38
_cell_volume                     5096.0(5)
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture Photon II CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Incoatec HeliosTM multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       68
_diffrn_reflns_limit_h_min       -68
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            53532
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.314
_diffrn_reflns_theta_min         2.382
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.310
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1345 before and 0.0678 after correction.
The Ratio of minimum to maximum transmission is 0.7491.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         6331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+8.4208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1025
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5887
_reflns_number_total             6331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce01136a2.cif
_cod_data_source_block           32108201_0m
_cod_original_cell_volume        5096.1(5)
_cod_database_code               7251500
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.942
_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:
 C7A(H7AA,H7AB), C8A(H8AA,H8AB), C7B(H7BA,H7BB), C8B(H8BA,H8BB)
2.b Me refined with riding coordinates:
 C21A(H21A,H21B,H21C), C21B(H21D,H21E,H21F)
2.c Aromatic/amide H refined with riding coordinates:
 C5A(H5A), C6A(H6A), C10A(H10A), C12A(H12A), C5B(H5B), C6B(H6B), C10B(H10B),
 C12B(H12B)
;
_shelx_res_checksum              53832
_olex2_submission_special_instructions 'No special instructions were received'