Exploring Desolvation-Driven Polymorph Formation via Multicomponent Crystals of Furosemide
Nomnganga, Yamkela; Oluwole, David O.; Venter, Gerhard A.; Benyei, Attila; Bathori, Nikoletta B.; CrystEngComm  (2025) –; doi:10.1039/D5CE01033K

data_7251389
_publ_section_title
;
 Exploring Desolvation-Driven Polymorph Formation via Multicomponent
 Crystals of Furosemide
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D5CE01033K
_journal_year                    2025
_chemical_formula_moiety         'C12 H10 Cl N2 O5 S, C7 H10 N'
_chemical_formula_sum            'C19 H20 Cl N3 O5 S'
_chemical_formula_weight         437.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-09-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_audit_update_record
;
2025-08-05 deposited with the CCDC.	2025-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.7990(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1621(7)
_cell_length_b                   9.6366(5)
_cell_length_c                   14.7725(7)
_cell_measurement_reflns_used    5561
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.589
_cell_measurement_theta_min      1.828
_cell_volume                     1980.37(17)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  Bruker
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0124
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            50795
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.589
_diffrn_reflns_theta_min         1.828
_exptl_absorpt_coefficient_mu    0.336
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.7189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       chunk
_exptl_crystal_F_000             912
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 2,3-dimethyl-pyridine'
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.172
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         5561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0399P)^2^+1.0162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5185
_reflns_number_total             5561
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce01033k2.cif
_cod_data_source_block           FUR23LUT
_cod_database_code               7251389
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.915
_exptl_absorpt_special_details
'Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D. J. Appl. Cryst. 48 (2015) 3-10.'
_olex2_refinement_description
;
1.a Riding coordinates:
 N1(H1B,H1A), N2(H2), N3(H4)
1.b Secondary CH2 refined with riding coordinates:
 C8(H8B,H8A)
1.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16), C17(H17)
1.d Idealised Me refined as rotating group:
 C18(H18A,H18C,H18B), C19(H19C,H19B,H19A)
;
_shelx_res_checksum              71514
_olex2_submission_special_instructions 'No special instructions were received'