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_3000604
_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'
_chemical_formula_sum            'C7 H6 O4'
_chemical_formula_weight         154.12
_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     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                90
_cell_angle_beta                 99.801(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.6740(6)
_cell_length_b                   22.230(2)
_cell_length_c                   8.0598(8)
_cell_measurement_reflns_used    8916
_cell_measurement_temperature    79
_cell_measurement_theta_max      1.2593825225381257
_cell_measurement_theta_min      0.13283470852102497
_cell_volume                     648.66(14)
_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 0.987
_diffrn_measured_fraction_theta_max 0.991
_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  0.2938
_diffrn_reflns_av_unetI/netI     0.1901
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            43188
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        0.862
_diffrn_reflns_theta_max         1.197
_diffrn_reflns_theta_min         0.133
_diffrn_source                   'Talos Arctica Field Emission Gun'
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       powder
_exptl_crystal_F_000             112
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       85926(9)
_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   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         3114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.2006
_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^)+(0.1654P)^2^+0.0891P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4061
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2013
_reflns_number_total             3114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            24DHBA.cif
_cod_data_source_block           24dhba
_cod_depositor_comments
;Releasing structure 3000604 into public domain as published material by
 including journal information.
;
_cod_original_cell_volume        648.65(14)
_cod_database_code               3000604
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C3(H3)
2.b Idealised tetrahedral OH refined as rotating group:
 O11(H11), O10(H10), O8(H8)
;
_shelx_res_checksum              48486
_shelx_hkl_checksum              45801
_olex2_submission_special_instructions 'No special instructions were received'