Microcrystal electron diffraction (MicroED) structure determination of a mechanochemically synthesized co-crystal not affordable from solution crystallization
Sasaki, Toshiyuki; Nakane, Takanori; Kawamoto, Akihiro; Nishizawa, Tomohiro; Kurisu, Genji; CrystEngComm  (2023) –; doi:10.1039/D2CE01522F

data_3000424
_publ_section_title
;
 Microcrystal electron diffraction (MicroED) structure determination of a
 mechanochemically synthesized co-crystal not affordable from solution
 crystallization
;
_journal_name_full               CrystEngComm
_journal_page_first              'not assigned yet (2023-01-10)'
_journal_paper_doi               10.1039/D2CE01522F
_journal_year                    2023
_chemical_formula_moiety         'C4 H5 N3, C2 H3 O2'
_chemical_formula_sum            'C6 H8 N3 O2'
_chemical_formula_weight         154.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-07-25
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-10-06 deposited with the CCDC.	2022-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.67
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.759
_cell_length_b                   5.200
_cell_length_c                   12.760
_cell_measurement_reflns_used    2923
_cell_measurement_temperature    79
_cell_measurement_theta_max      1.02465176988461
_cell_measurement_theta_min      0.14661895733917485
_cell_volume                     713.832
_computing_cell_refinement
'dials.two_theta_refine (Waterman et al., 2016)'
_computing_data_collection
'Verlox (Thermo Fisher Scientific) and 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_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
Talos Arctica G2
;
_diffrn_radiation_type           electrons
_diffrn_radiation_wavelength     0.02508
_diffrn_reflns_av_R_equivalents  0.3296
_diffrn_reflns_av_unetI/netI     0.2018
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38658
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        0.862
_diffrn_reflns_theta_max         1.026
_diffrn_reflns_theta_min         0.149
_diffrn_source                   electrons
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       platelet
_exptl_crystal_F_000             117
_exptl_crystal_recrystallization_method Co-grinding
_refine_diff_density_max         0.157
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       19793(20)
_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   1.026
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         2172
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1822
_refine_ls_R_factor_gt           0.1120
_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^)+(0.1583P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2990
_refine_ls_wR_factor_ref         0.3195
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                964
_reflns_number_total             2172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2211429.cif
_cod_data_source_block           cocrystal
_cod_depositor_comments
;Author list has been updated.

 Releasing structure 3000424 into public domain as published material.
;
_cod_original_cell_volume        713.8
_cod_database_code               3000424
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.01
2. 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
;
_shelx_res_checksum              4552
_shelx_hkl_checksum              9548
_olex2_submission_special_instructions 'No special instructions were received'