A single crystal to single crystal solvatomorphic phase transition in cocrystals of pyrimethamine with 4-hydroxybenzoic acid. An experimental and theoretical study
Bilal, Aqsa; Mehmood, Arshad; Noureen, Sajida; Ahmed, Maqsood; CrystEngComm 27 (2025) 4722–4733; doi:10.1039/D5CE00243E

data_7250471
_publ_section_title
;
 A single crystal to single crystal solvatomorphic phase transition in
 cocrystals of pyrimethamine with 4-hydroxybenzoic acid. An experimental
 and theoretical study
;
_journal_issue                   27
_journal_name_full               CrystEngComm
_journal_page_first              4722
_journal_page_last               4733
_journal_paper_doi               10.1039/D5CE00243E
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C12 H14 Cl N4, C7 H5 O3, H2 O '
_chemical_formula_sum            'C19 H21 Cl N4 O4'
_chemical_formula_weight         404.830
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'MoPro v21.06             '
_audit_update_record
;
2025-05-08 deposited with the CCDC.	2025-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.
_cell_angle_beta                 97.994(2)
_cell_angle_gamma                90.
_cell_formula_units_Z            8
_cell_length_a                   16.4563(6)
_cell_length_b                   14.2010(6)
_cell_length_c                   16.4360(8)
_cell_measurement_reflns_used    3865
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2.2
_cell_volume                     3803.7(3)
_computing_cell_refinement       'SAINT V8.40B (2016)'
_computing_data_collection
'Bruker BIS V6.2.16/2021-10-23 and APEX4 2022.1-1'
_computing_data_reduction        'SAINT V8.40B (2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'MoPro (J. Appl. Cryst. 2005, 38, 38-54)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.526
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.062
_diffrn_reflns_av_sigmaI/netI    0.05111
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3865
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    0.235
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.697
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0977 before and 0.0611 after correction.
The Ratio of minimum to maximum transmission is 0.9345.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.39
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3865
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.000
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'calc w =1/[2.6628*\s^2^(Fo^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0678
_reflns_number_gt                2633
_reflns_number_total             3865
_reflns_threshold_expression     'I > 2 \s(I)'
_publcif_datablock.id            {dfb70316-336d-43a2-826b-5fa161fde704}
_cod_data_source_file            d5ce00243e2.cif
_cod_data_source_block           IAM_MoPro
_cod_depositor_comments
'Adding full bibliography for 7250470--7250473.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7250471
_symmetry_space_group_name_h-m_alt C2/c