Pharmaceutical salts to improve diffusion permeability of a BCS class III β-blocker drug atenolol
Shajan, Daliya K.; Pandey, Noopur; Ghosh, Animesh; Srivastava, Anubha; Sanphui, Palash; CrystEngComm 26 (2024) 6420–6431; doi:10.1039/D4CE01003E

data_7249472
_publ_section_title
;
 Pharmaceutical salts to improve diffusion permeability of a BCS class III
 \b-blocker drug atenolol
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              6420
_journal_page_last               6431
_journal_paper_doi               10.1039/D4CE01003E
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C14 H23 N2 O3, C2 H O2, H2 O'
_chemical_formula_sum            'C16 H26 N2 O6'
_chemical_formula_weight         342.39
_chemical_name_systematic        'Atenolol fumarate 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'
_symmetry_Int_Tables_number      14
_audit_creation_date             2022-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-12-17 deposited with the CCDC.	2024-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.1970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6451(3)
_cell_length_b                   9.4203(3)
_cell_length_c                   17.2278(4)
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.48
_cell_volume                     1805.41(9)
_computing_cell_refinement       'SAINT V8.40E (?, 2016)'
_computing_data_reduction        'SAINT V8.40E (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.9951
_diffrn_measured_fraction_theta_max 0.9951
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            38976
_diffrn_reflns_theta_full        28.3521
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         2.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6839
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0642 before and 0.0506 after correction.
The Ratio of minimum to maximum transmission is 0.9171.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.2596
_exptl_crystal_description       block
_exptl_crystal_F_000             736.4384
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetone-methanol mixture'
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.6879
_refine_diff_density_min         -0.2259
_refine_diff_density_rms         0.0470
_refine_ls_d_res_high            0.7483
_refine_ls_d_res_low             8.2288
_refine_ls_goodness_of_fit_ref   1.0452
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    37
_refine_ls_number_parameters     231
_refine_ls_number_reflns         4496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0452
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+0.9320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1579
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                3976
_reflns_number_total             4496
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4ce01003e2.cif
_cod_data_source_block           ATL-FMA_hyd
_cod_depositor_comments          'Adding full bibliography for 7249472.cif.'
_cod_database_code               7249472
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C12(H12)
2.b Secondary CH2 refined with riding coordinates:
 N2(H2a,H2b), C2(H2c,H2d), C9(H9a,H9b), C11(H11a,H11b)
2.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C4(H4), C5(H5), C7(H7), C8(H8)
2.d X=CH2 refined with riding coordinates:
 N1(H1a,H1b)
2.e Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C13(H13a,H13b,H13c)
;
_olex2_submission_special_instructions 'No special instructions were received'