Solid-state conformations of pharmaceutical polymorphs in solution: validation and invalidation by NMR.
Joshi, Kirthi; Sangwan, Shruti; Jose, K. V. Jovan; Agarwal, Vipin.; Nangia, Ashwini K.; CrystEngComm 28 (2026) 1339–1350; doi:10.1039/D5CE01120E

data_7251490
_publ_section_title
;
 Solid-state conformations of pharmaceutical polymorphs in solution:
 validation and invalidation by NMR.
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              1339
_journal_page_last               1350
_journal_paper_doi               10.1039/D5CE01120E
_journal_volume                  28
_journal_year                    2026
_chemical_formula_moiety         'C17 H21 N3 O S'
_chemical_formula_sum            'C17 H21 N3 O S'
_chemical_formula_weight         315.43
_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   geom
_audit_creation_date             2025-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-03-13 deposited with the CCDC.	2026-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.325(5)
_cell_length_b                   12.993(6)
_cell_length_c                   16.832(11)
_cell_measurement_reflns_used    2559
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      0.975
_cell_measurement_theta_min      0.928
_cell_volume                     1602.0(17)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    %$getVar(solution_reference_short)%
_diffrn_ambient_temperature      296.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1384
_diffrn_reflns_av_unetI/netI     0.0842
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            51627
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.129
_diffrn_reflns_theta_min         1.980
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'metallic light yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       plate
_exptl_crystal_F_000             672
_exptl_crystal_preparation       'heat cool heat'
_exptl_crystal_recrystallization_method 'from form 1b'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 800 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.47(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3803
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0634
_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^)+(0.0746P)^2^+0.3153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1458
_refine_ls_wR_factor_ref         0.1654
_reflns_Friedel_coverage         0.734
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                2559
_reflns_number_total             3803
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce01120e2.cif
_cod_data_source_block           an184_0m
_cod_depositor_comments
'Adding full bibliography for 7251488--7251490.cif.'
_cod_original_cell_volume        1602.1(16)
_cod_database_code               7251490
_shelx_shelxl_version_number     2014/7
_publ_section_exptl
;
Any special experimental details
;
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.929
_olex2_refinement_description
;
1. 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
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C4(H4A,H4B), C3(H3A,H3B), C1(H1A,H1B), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C11(H11), C9(H9), C14(H14), C15(H15)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C16(H16A,H16B,H16C)
;
_olex2_submission_special_instructions 'No special instructions were received'