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_7251498
_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         'C8 H11 N O5 S, H2 O'
_chemical_formula_sum            'C8 H13 N O6 S'
_chemical_formula_weight         251.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-11-24 deposited with the CCDC.	2026-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8391(3)
_cell_length_b                   11.2218(5)
_cell_length_c                   13.7253(6)
_cell_measurement_reflns_used    9130
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      68.29
_cell_measurement_theta_min      3.22
_cell_volume                     1053.38(8)
_computing_cell_refinement       'Bruker Apex4, 2021'
_computing_data_collection       'Bruker Apex4, 2021'
_computing_data_reduction        'SAINT v8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2-1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2-1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24647
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.285
_diffrn_reflns_theta_min         5.091
_diffrn_source                   'high brilliance microfocus sealed tube'
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.922
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.4148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1561 before and 0.0869 after correction.
The Ratio of minimum to maximum transmission is 0.5508.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       prism
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.17(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         1890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0354P)^2^+0.4518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0677
_reflns_Friedel_coverage         0.671
_reflns_Friedel_fraction_full    0.960
_reflns_Friedel_fraction_max     0.961
_reflns_number_gt                1890
_reflns_number_total             1890
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce01136a2.cif
_cod_data_source_block           1
_cod_database_code               7251498
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.636
_shelx_estimated_absorpt_t_min   0.329
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.83(2)
 0.17(2)
2. 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, All O(H) groups, All O(H,H) groups
3.a Free rotating group:
 O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
3.c Aromatic/amide H refined with riding coordinates:
 C5C(H5C), C6C(H6C)
3.d Idealised Me refined as rotating group:
 C21C(H21A,H21B,H21C)
3.e Idealised tetrahedral OH refined as rotating group:
 O31C(H31C), O41C(H41C)
;
_shelx_res_checksum              88721
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_special_instructions 'No special instructions were received'