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_7251806
_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, C3 H5 N2'
_chemical_formula_sum            'C21 H18 N6 O5 S'
_chemical_formula_weight         466.478
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_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
;
2026-03-11 deposited with the CCDC.	2026-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                80.405(7)
_cell_angle_beta                 86.616(9)
_cell_angle_gamma                88.202(7)
_cell_formula_units_Z            4
_cell_length_a                   8.1244(9)
_cell_length_b                   10.3705(8)
_cell_length_c                   26.277(2)
_cell_measurement_reflns_used    4759
_cell_measurement_temperature    175(5)
_cell_measurement_theta_max      0.7770
_cell_measurement_theta_min      0.0250
_cell_volume                     2178.6(3)
_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 0.9882
_diffrn_measured_fraction_theta_max 0.9882
_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    -60.00  39.25   0.25    0.50    --    0.00   0.00   0.00  397
  2  \w    -55.00  55.00   0.25    0.50    --    0.00   0.00   0.00  440
  3  \w    -45.00  62.00   0.25    0.50    --    0.00   0.00   0.00  428
  4  \w    -55.00  60.00   0.25    1.00    --    0.00   0.00   0.00  460
  5  \w    -60.00  50.00   0.25    0.75    --    0.00   0.00   0.00  440
  6  \w    -60.00  45.00   0.25    0.75    --    0.00   0.00   0.00  420
;
_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      0.0030956000
_diffrn_orient_matrix_UB_12      -0.0000541000
_diffrn_orient_matrix_UB_13      -0.0000528000
_diffrn_orient_matrix_UB_21      0.0000005000
_diffrn_orient_matrix_UB_22      0.0024547000
_diffrn_orient_matrix_UB_23      -0.0001618000
_diffrn_orient_matrix_UB_31      -0.0000005000
_diffrn_orient_matrix_UB_32      0.0000008000
_diffrn_orient_matrix_UB_33      0.0009552000
_diffrn_radiation_monochromator  none
_diffrn_radiation_probe          electron
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.0251
_diffrn_reflns_av_R_equivalents  0.2482
_diffrn_reflns_av_unetI/netI     0.1578
_diffrn_reflns_Laue_measured_fraction_full 0.9882
_diffrn_reflns_Laue_measured_fraction_max 0.9882
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27737
_diffrn_reflns_point_group_measured_fraction_full 0.9882
_diffrn_reflns_point_group_measured_fraction_max 0.9882
_diffrn_reflns_theta_full        0.7190
_diffrn_reflns_theta_max         0.72
_diffrn_reflns_theta_min         0.07
_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            'orange (bulk)'
_exptl_crystal_colour_primary    'orange (bulk'
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       irregular
_exptl_crystal_F_000             362.068
_exptl_crystal_preparation
;
sample ground gently between glass slides, grid dabbed in solid, cryo-transfer
at 175(5) K
;
_exptl_crystals_number           6
_refine_ls_d_res_high            1.0001
_refine_ls_d_res_low             10.2230
_refine_ls_extinction_coef       74(26)
_refine_ls_extinction_expression
;
Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
;
_refine_ls_goodness_of_fit_ref   1.0157
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    59
_refine_ls_number_parameters     631
_refine_ls_number_reflns         4505
_refine_ls_number_restraints     540
_refine_ls_restrained_S_all      0.9516
_refine_ls_R_factor_all          0.1995
_refine_ls_R_factor_gt           0.1325
_refine_ls_shift/su_max          -0.0006
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.3000P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3723
_refine_ls_wR_factor_ref         0.4243
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              10
_reflns_limit_k_min              -10
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                2579
_reflns_number_total             4505
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5ce01188d2.cif
_cod_data_source_block           SSZ-IMID
_cod_depositor_comments
'Adding full bibliography for 7251806--7251807.cif.'
_cod_original_cell_volume        2178.7(3)
_cod_database_code               7251806
_chemical_oxdiff_formula         'C18H14N4O5S C3H4N2'
_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        43467f85a962607acb3e409c82d631f08d81ae
_diffrn_oxdiff_digest_hkl_ed     53a3453125bbb7863ef53df8c478599b5a9f79
_diffrn_oxdiff_measurement_exp_name m_971_973_974_978_980_981.par
_diffrn_source_make              'JEOL JEM-2300ED, LaB6'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 C24-C25 = C25-C26 = C26-C27 = C27-C28 = C28-C29 = C29-C24
 1.39 with sigma of 0.01
 C30-C31 = C31-C32 = C32-C33 = C33-C34 = C34-C35 = C35-C30
 1.39 with sigma of 0.01
 C12-C13 = C13-C14 = C14-C15 = C15-C16 = C16-C17 = C17-C12
 1.39 with sigma of 0.01
 C6-C7 = C7-C8 = C8-C9 = C9-C10 = C10-C11 = C11-C6
 1.39 with sigma of 0.01
 C24-C26 \\sim C25-C27 \\sim C26-C28 \\sim C27-C29 \\sim C28-C24 \\sim C29-C25
 with sigma of 0.02
 C30-C32 \\sim C31-C33 \\sim C32-C34 \\sim C33-C35 \\sim C34-C30 \\sim C35-C31
 with sigma of 0.02
 C12-C14 \\sim C13-C15 \\sim C14-C16 \\sim C15-C17 \\sim C16-C12 \\sim C17-C13
 with sigma of 0.02
 C6-C8 \\sim C7-C9 \\sim C8-C10 \\sim C9-C11 \\sim C10-C6 \\sim C11-C7
 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
4. Others
 Sof(H6)=1-FVAR(1)
 Sof(H5)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5b), C7(H7), C8(H8), C10(H10a), C11(H11),
 C13(H13), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25),
  C26(H26), C28(H28), C29(H29), C31(H31), C34(H34), C35(H35), C37(H37),
 C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
;
_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 4.584
_oxdiff_exptl_absorpt_empirical_full_min 0.342
_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       0.9289
_refine_diff.potential_min       -0.8363
_refine_diff.potential_rms       0.2105