High-throughput co-former screening and structural elucidation using resonant acoustic mixing and 3D electron diffraction
Danks, Jacob; Rainer, Daniel N.; Hamza, Ahmed S.; Coles, Simon J.; Carter, Anthony B.; Benson, Joseph E. G.; CrystEngComm 28 (2026) 2018–2022; doi:10.1039/D5CE01188D

data_7251807
_publ_section_title
;
 High-throughput co-former screening and structural elucidation using
 resonant acoustic mixing and 3D electron diffraction
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              2018
_journal_page_last               2022
_journal_paper_doi               10.1039/D5CE01188D
_journal_volume                  28
_journal_year                    2026
_chemical_formula_moiety         'C18 H13 N4 O5 S, C5 H7 N2'
_chemical_formula_sum            'C23 H20 N6 O5 S'
_chemical_formula_weight         492.516
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_Int_Tables_number      13
_atom_sites_solution_primary     dual
_audit_creation_date             2025-11-11
_audit_creation_method
;
Olex2 1.5-ac7-018
(compiled 2025.08.06 svn.rb7424aed for Rigaku Oxford Diffraction, GUI svn.r7314)

CIVET v1.2 (Daniel N. Rainer, https://github.com/danielnrainer/CIVET)
;
_audit_update_record
;
2026-03-06 deposited with the CCDC.	2026-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.129(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4997(19)
_cell_length_b                   6.2871(3)
_cell_length_c                   19.695(2)
_cell_measurement_reflns_used    8852
_cell_measurement_temperature    175(5)
_cell_measurement_theta_max      0.8920
_cell_measurement_theta_min      0.0460
_cell_volume                     2319.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.44.127a (Rigaku OD, 2025)'
_computing_data_collection
;
CrysAlisPro system (CCD 44.47a 64-bit (release 24-04-2024))
;
_computing_data_reduction        'CrysAlisPro 1.171.44.127a (Rigaku OD, 2025)'
_computing_molecular_graphics    'Olex2 1.5-ac7-018 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac7-018 (Dolomanov et al., 2009)'
_computing_structure_refinement
;
olex2.refine 1.5-ac7-018 (Bourhis et al., 2015)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      vacuum
_diffrn_ambient_temperature      175(5)
_diffrn_detector                 'hybrid pixel array detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'Rigaku HyPix-ED'
_diffrn_measured_fraction_theta_full 0.9786
_diffrn_measured_fraction_theta_max 0.9781
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -52.50  55.00   0.25    0.50    --    0.00   0.00   0.00  430
  2  \w    -60.00  40.00   0.25    0.50    --    0.00   0.00   0.00  400
  3  \w    -30.25  60.00   0.25    0.50    --    0.00   0.00   0.00  361
  4  \w    -55.00  55.00   0.25    0.50    --    0.00   0.00   0.00  440
  5  \w    -62.00  45.00   0.25    0.50    --    0.00   0.00   0.00  428
;
_diffrn_measurement_device       'electron diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-ED'
_diffrn_measurement_method       'continuous rotation electron diffraction'
_diffrn_measurement_specimen_support 'holey carbon copper grid, 200 mesh'
_diffrn_orient_matrix_type
;
CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      0.0013389000
_diffrn_orient_matrix_UB_12      -0.0000075000
_diffrn_orient_matrix_UB_13      0.0003649000
_diffrn_orient_matrix_UB_21      0.0000004000
_diffrn_orient_matrix_UB_22      0.0039943000
_diffrn_orient_matrix_UB_23      0.0000021000
_diffrn_orient_matrix_UB_31      0.0000006000
_diffrn_orient_matrix_UB_32      -0.0000016000
_diffrn_orient_matrix_UB_33      0.0012749000
_diffrn_radiation_monochromator  none
_diffrn_radiation_probe          electron
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.0251
_diffrn_reflns_av_R_equivalents  0.1838
_diffrn_reflns_av_unetI/netI     0.1105
_diffrn_reflns_Laue_measured_fraction_full 0.9786
_diffrn_reflns_Laue_measured_fraction_max 0.9781
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32661
_diffrn_reflns_point_group_measured_fraction_full 0.9786
_diffrn_reflns_point_group_measured_fraction_max 0.9781
_diffrn_reflns_theta_full        0.8629
_diffrn_reflns_theta_max         0.90
_diffrn_reflns_theta_min         0.05
_diffrn_source                   'electron gun'
_diffrn_source_size
;
SAED nominal aperture diameter 100 um, corresponding to a diameter of about 2 um
at the image plane.
;
_diffrn_source_voltage           200
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'white (bulk)'
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       irregular
_exptl_crystal_F_000             386.356
_exptl_crystal_preparation
;
sample ground gently between glass slides, grid dabbed in solid, cryo-transfer
at 175(5) K
;
_exptl_crystals_number           5
_refine_ls_d_res_high            0.8001
_refine_ls_d_res_low             15.6635
_refine_ls_extinction_coef       512(59)
_refine_ls_extinction_expression
;
Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
;
_refine_ls_goodness_of_fit_ref   1.0532
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    32
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4636
_refine_ls_number_restraints     285
_refine_ls_restrained_S_all      1.0199
_refine_ls_R_factor_all          0.1908
_refine_ls_R_factor_gt           0.1499
_refine_ls_shift/su_max          -0.0008
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.1779P)^2^+0.8633P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3812
_refine_ls_wR_factor_ref         0.4054
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -24
_reflns_limit_k_max              7
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              -14
_reflns_number_gt                3081
_reflns_number_total             4636
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5ce01188d2.cif
_cod_data_source_block           SSZ-AMIN
_cod_depositor_comments
'Adding full bibliography for 7251806--7251807.cif.'
_cod_original_cell_volume        2319.4(4)
_cod_database_code               7251807
_chemical_oxdiff_formula         'C18H14N4O5S C5H6N2'
_chemical_oxdiff_usercomment
;
Agar holey carbon grid, sample ground between glass slides, grid tapped, cryo
transfer @ 175 K, coll @ 175 K
;
_diffrn_oxdiff_scatteringfactors_ed
;
UCLA (2022) https://srv.mbi.ucla.edu/faes/data
;
_diffrn_oxdiff_digest_creation   'CAP 1.171.44.127a, AC 1.5-ac7-018'
_diffrn_oxdiff_digest_hkl        4307ff630c027a1a2ccb5447b9ab58eaed8735
_diffrn_oxdiff_digest_hkl_ed     537bc791a0940279b67c44eb51826c067637c1
_diffrn_oxdiff_measurement_exp_name m_983_987_989_990_991.par
_diffrn_source_make              'JEOL JEM-2300ED, LaB6'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H) groups
2. Restrained distances
 C15-C14 = C14-C13 = C13-C12 = C12-C17 = C17-C16 = C16-C15
 1.39 with sigma of 0.01
 C7-C6 = C6-C11 = C11-C10 = C10-C9 = C9-C8 = C8-C7
 1.39 with sigma of 0.01
 C15-C13 \\sim C14-C12 \\sim C13-C17 \\sim C12-C16 \\sim C17-C15 \\sim C16-C14
 with sigma of 0.02
 C7-C11 \\sim C6-C10 \\sim C11-C9 \\sim C10-C8 \\sim C9-C7 \\sim C8-C6
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C2(H2), C3(H3), C4(H4), C7(H7), C13(H13), C8(H8), C11(H11), C10(H10),
 C16(H16), C23(H23), C22(H22), C17(H17), C20(H20), C21(H21)
;
_olex2_submission_special_instructions
;
No special instructions were received
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.047
_oxdiff_exptl_absorpt_empirical_full_min 0.245
_diffrn_source.ed_diffracting_area_selection SAED
_diffrn_measurement.rotation_mode rotation
_refine.diffraction_theory       kinematical
_diffrn_measurement.sample_tracking no
_diffrn_radiation.illumination_mode parallel
_diffrn_measurement.method_precession no
_refine_diff.potential_max       1.4940
_refine_diff.potential_min       -0.9060
_refine_diff.potential_rms       0.1792