Structural landscape of new salts of the antihistamine drug bilastine: implications in physicochemical properties and anticancer activity against skin cancer
Kanagavel, Manimurugan; Sparjan Samuvel, Rajan Marystella; Ramalingam, Vaikundamoorthy; Nechipadappu, Sunil Kumar; CrystEngComm 27 (2025) 2317–2332; doi:10.1039/D4CE01303D

data_1574148
_publ_section_title
;
 Structural landscape of new salts of the antihistamine drug bilastine:
 implications in physicochemical properties and anticancer activity
 against skin cancer
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              2317
_journal_page_last               2332
_journal_paper_doi               10.1039/D4CE01303D
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C28 H39 N3 O3, 2(H O4 S), 3(H2 O), O'
_chemical_formula_sum            'C28 H47 N3 O15 S2'
_chemical_formula_weight         729.80
_chemical_name_common            'BILASTINE DI SULFATE TETRA HYDRATE'
_chemical_name_systematic        'BILASTINE DI SULFATE TETRA HYDRATE'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-07-27 deposited with the CCDC.	2025-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.259(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8559(11)
_cell_length_b                   34.775(3)
_cell_length_c                   8.4372(8)
_cell_measurement_reflns_used    6365
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.6
_cell_measurement_theta_min      2.46
_cell_volume                     3478.5(6)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2016)'
_computing_data_collection       '<i>APEX3</i> (Bruker, 2016)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  '<i>SHELXL2014</i> (Sheldrick, 2015)'
_computing_structure_solution    '<i>SHELXT</i> (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON-III'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0932
_diffrn_reflns_av_unetI/netI     0.0891
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            28452
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.171
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.2629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       needle
_exptl_crystal_F_000             1552
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.0065(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         5986
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0806
_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^)+(0.0248P)^2^+13.3707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1755
_refine_ls_wR_factor_ref         0.1958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4041
_reflns_number_total             5986
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01303d2.cif
_cod_data_source_block           KB1028_0m_a
_cod_depositor_comments
'Adding full bibliography for 1574143--1574149.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1574148
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.956
_shelx_estimated_absorpt_t_max   0.976
_shelx_res_checksum              83798