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_7251499
_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         'C22 H26 Cu N6 O4, 2(Cl), 4(H2 O)'
_chemical_formula_sum            'C22 H34 Cl2 Cu N6 O8'
_chemical_formula_weight         644.99
_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     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                94.856(2)
_cell_angle_beta                 103.393(2)
_cell_angle_gamma                103.024(2)
_cell_formula_units_Z            1
_cell_length_a                   8.1875(5)
_cell_length_b                   8.7569(5)
_cell_length_c                   9.8704(6)
_cell_measurement_reflns_used    9735
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.94
_cell_volume                     663.70(7)
_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  0.0388
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            31377
_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         28.315
_diffrn_reflns_theta_min         2.143
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.083
_exptl_absorpt_correction_T_max  0.4920
_exptl_absorpt_correction_T_min  0.4033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1357 before and 0.0526 after correction.
The Ratio of minimum to maximum transmission is 0.8197.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             335
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.123
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0222
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+0.3749P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0584
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3273
_reflns_number_total             3289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce01136a2.cif
_cod_data_source_block           32108202_0m
_cod_original_cell_volume        663.69(7)
_cod_database_code               7251499
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.835
_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:
 C7(H7A,H7B), C8(H8A,H8B)
2.b Me refined with riding coordinates:
 C21(H21A,H21B,H21C)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C10(H10), C12(H12)
;
_shelx_res_checksum              56143
_olex2_submission_special_instructions 'No special instructions were received'