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_3000605
_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         '2(C H4 N2 O), C7 H6 O4'
_chemical_formula_sum            'C9 H14 N4 O6'
_chemical_formula_weight         274.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-09
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                74.412(15)
_cell_angle_beta                 75.956(14)
_cell_angle_gamma                71.464(14)
_cell_formula_units_Z            2
_cell_length_a                   7.2558(10)
_cell_length_b                   8.8651(16)
_cell_length_c                   10.860(2)
_cell_measurement_reflns_used    8666
_cell_measurement_temperature    79
_cell_measurement_theta_max      1.1171058736815767
_cell_measurement_theta_min      0.13786914567765718
_cell_volume                     628.4(2)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      79
_diffrn_detector
;
Falcon 3 direct electron camera (integration mode)
;
_diffrn_detector_type            CMOS
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.996
_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  0.2278
_diffrn_reflns_av_unetI/netI     0.1231
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            47366
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        0.862
_diffrn_reflns_theta_max         0.984
_diffrn_reflns_theta_min         0.116
_diffrn_source                   'Talos Arctica Field Emission Gun'
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       powder
_exptl_crystal_F_000             99
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       21014(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   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3360
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.1927
_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^)+(0.1554P)^2^+0.2722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4008
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2195
_reflns_number_total             3360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Urea-24DHBA-Pre.cif
_cod_data_source_block           urea-24dhba-pre
_cod_depositor_comments
;Releasing structure 3000605 into public domain as published material by
 including journal information.
;
_cod_database_code               3000605
_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. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.05 and sigma for 1-3 distances of 0.05
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C3(H3)
4.b X=CH2 refined with riding coordinates:
 N14(H14A,H14B), N15(H15A,H15B), N18(H18A,H18B), N19(H19A,H19B)
4.c Idealised tetrahedral OH refined as rotating group:
 O11(H11), O9(H9), O10(H10)
;
_shelx_res_checksum              42328
_shelx_hkl_checksum              88140
_olex2_submission_special_instructions 'No special instructions were received'