Beyond serendipity: uncovering novel ratiometric urea-24DHBA cocrystals through mechanochemistry and MicroED
Bania, Ankur; Gogoi, Diptajyoti; Kalita, Nabadeep; Nakane, Takanori; Kawamoto, Akihiro; Althubeiti, Khaled; Sasaki, Toshiyuki; Kurisu, Genji; Thakuria, Ranjit; Chemical Communications 61 (2025) 16198–16201; doi:10.1039/D5CC03628C

data_3000606
_publ_section_title
;
 Beyond serendipity: uncovering novel ratiometric urea-24DHBA cocrystals
 through mechanochemistry and MicroED
;
_journal_name_full               'Chemical Communications'
_journal_page_first              16198
_journal_page_last               16201
_journal_paper_doi               10.1039/D5CC03628C
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C7 H6 O4, C H4 N2 O'
_chemical_formula_sum            'C8 H10 N2 O5'
_chemical_formula_weight         214.18
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-06-10
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.70(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   6.9711(15)
_cell_length_b                   11.059(3)
_cell_length_c                   31.307(7)
_cell_measurement_reflns_used    4205
_cell_measurement_temperature    79
_cell_measurement_theta_max      0.8684896833716158
_cell_measurement_theta_min      0.12253341769976006
_cell_volume                     2412.5(10)
_computing_cell_refinement
'dials.two_theta_refine (Waterman et al., 2016)'
_computing_data_collection       'SerialEM (Mastronarde, 2005)'
_computing_data_reduction        'dials.scale (Beilsten-Edmands et al., 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      79
_diffrn_detector
;
Falcon 3 direct electron camera (integration mode)
;
_diffrn_detector_type            CMOS
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Talos Arctica electron microscope'
_diffrn_measurement_method
;
continuous rotation electron diffraction (MicroED)
;
_diffrn_radiation_probe          electron
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.02508
_diffrn_reflns_av_R_equivalents  0.3357
_diffrn_reflns_av_unetI/netI     0.0997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            78363
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        0.862
_diffrn_reflns_theta_max         0.866
_diffrn_reflns_theta_min         0.122
_diffrn_source                   'Talos Arctica Field Emission Gun'
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_description       powder
_exptl_crystal_F_000             310
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       9556(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.643
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         4413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.643
_refine_ls_R_factor_all          0.2208
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4599
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2923
_reflns_number_total             4413
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Urea-24DHBA-Post.cif
_cod_data_source_block           urea-24dhba-post
_cod_depositor_comments
;Releasing structure 3000606 into public domain as published material by
 including journal information.
;
_cod_original_cell_volume        2412.6(10)
_cod_database_code               3000606
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C6(H6), C17(H17), C5(H5), C3(H3), C16(H16)
2.b X=CH2 refined with riding coordinates:
 N29(H29A,H29B), N25(H25A,H25B), N26(H26A,H26B), N30(H30A,H30B)
2.c Idealised tetrahedral OH refined as rotating group:
 O10(H10), O21(H21), O20(H20), O11(H11), O22(H22), O9(H9)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              37805
_shelx_hkl_checksum              308
_shelx_fab_checksum              21020
_olex2_submission_special_instructions 'No special instructions were received'