Understanding the stability of the amorphous form of darifenacin
Nowak, Przemysław; Pietrzak, Anna; Dudek, Marta K.; CrystEngComm 27 (2025) 1927–1938; doi:10.1039/D4CE01257G

data_7249969
_publ_section_title
;
 Understanding the stability of the amorphous form of darifenacin
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              1927
_journal_page_last               1938
_journal_paper_doi               10.1039/D4CE01257G
_journal_volume                  27
_journal_year                    2025
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C28 H30 N2 O2, C7 H8'
_chemical_formula_sum            'C35 H38 N2 O2'
_chemical_formula_weight         518.67
_chemical_name_common            'darifenacin solvate with toluene'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     other
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-02-13 deposited with the CCDC.	2025-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.0220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.23630(10)
_cell_length_b                   8.78740(10)
_cell_length_c                   14.0356(2)
_cell_measurement_reflns_used    27399
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      76.4500
_cell_measurement_theta_min      3.4140
_cell_volume                     1388.98(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2019)'
_diffrn_ambient_temperature      99.99(10)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37677
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.919
_diffrn_reflns_theta_min         3.421
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       plate
_exptl_crystal_F_000             556
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.181
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 2092 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.11(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         5409
_refine_ls_number_restraints     213
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0325P)^2^+0.7647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.0971
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.878
_reflns_number_gt                5106
_reflns_number_total             5409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01257g2.cif
_cod_data_source_block           exp_143_cut_Rint
_cod_depositor_comments
'Adding full bibliography for 7249968--7249969.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7249969
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.880
_shelx_estimated_absorpt_t_max   0.977
_oxdiff_exptl_absorpt_empirical_full_min 0.612
_oxdiff_exptl_absorpt_empirical_full_max 2.724
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_shelx_res_checksum              78074