Structure determination of small molecule compounds by an electron diffractometer for 3D ED/MicroED
Ito, Sho; White, Fraser J.; Okunishi, Eiji; Aoyama, Yoshitaka; Yamano, Akihito; Sato, Hiroyasu; Ferrara, Joseph D.; Jasnowski, Michał; Meyer, Mathias; CrystEngComm 23 (2021) 8622–8630; doi:10.1039/D1CE01172C

data_7243941
_publ_section_title
;
 Structure determination of small molecule compounds by an electron
 diffractometer for 3D ED/MicroED
;
_journal_issue                   48
_journal_name_full               CrystEngComm
_journal_page_first              8622
_journal_page_last               8630
_journal_paper_doi               10.1039/D1CE01172C
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C18 H12 N6'
_chemical_formula_sum            'C18 H12 N6'
_chemical_formula_weight         312.34
_chemical_name_systematic        2,4,6-tripyridin-4-yl-1,3,5-triazine
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-31 deposited with the CCDC.	2021-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.81(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.507(10)
_cell_length_b                   11.432(7)
_cell_length_c                   11.114(9)
_cell_measurement_reflns_used    318
_cell_measurement_temperature    293
_cell_measurement_theta_max      0.7984
_cell_measurement_theta_min      0.1107
_cell_volume                     1615(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.13a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.13a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.13a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'Rigaku HyPix-ED area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.819
_diffrn_measured_fraction_theta_max 0.819
_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    -40.00  40.00   1.00    4.00    --    0.00   0.00   0.00   80
  2  \w    -40.00  40.00   1.00   10.00    --    0.00   0.00   0.00   80
  3  \w    -40.00  40.00   1.00    4.00    --    0.00   0.00   0.00   80
;
_diffrn_measurement_device       'Electron diffractometer'
_diffrn_measurement_device_type  Rigaku_Synergy-ED
_diffrn_measurement_method       'continuous rotation'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0015309000
_diffrn_orient_matrix_UB_12      0.0003912000
_diffrn_orient_matrix_UB_13      0.0019981000
_diffrn_orient_matrix_UB_21      0.0010030000
_diffrn_orient_matrix_UB_22      0.0008699000
_diffrn_orient_matrix_UB_23      -0.0013191000
_diffrn_orient_matrix_UB_31      -0.0007429000
_diffrn_orient_matrix_UB_32      0.0019776000
_diffrn_orient_matrix_UB_33      0.0001732000
_diffrn_radiation_probe          electron
_diffrn_radiation_type           '200 keV electrons'
_diffrn_radiation_wavelength     0.0251
_diffrn_reflns_av_R_equivalents  0.1547
_diffrn_reflns_av_unetI/netI     0.0971
_diffrn_reflns_Laue_measured_fraction_full 0.819
_diffrn_reflns_Laue_measured_fraction_max 0.819
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4853
_diffrn_reflns_point_group_measured_fraction_full 0.819
_diffrn_reflns_point_group_measured_fraction_max 0.819
_diffrn_reflns_theta_full        0.798
_diffrn_reflns_theta_max         0.798
_diffrn_reflns_theta_min         0.121
_diffrn_source                   'thermionic-emission electron gun'
_diffrn_source_type              LaB6
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       plate
_exptl_crystal_F_000             259
_exptl_crystal_size_max          0.0005
_exptl_crystal_size_mid          0.0005
_exptl_crystal_size_min          0.0002
_refine_diff_density_max         0.182
_refine_diff_density_min         -0.151
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.477
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         952
_refine_ls_number_restraints     222
_refine_ls_restrained_S_all      2.392
_refine_ls_R_factor_all          0.2375
_refine_ls_R_factor_gt           0.1900
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4192
_refine_ls_wR_factor_ref         0.4328
_reflns_Friedel_coverage         0.000
_reflns_number_gt                616
_reflns_number_total             952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01172c1.cif
_cod_data_source_block           5_11_14
_cod_depositor_comments
'Adding full bibliography for 7243939--7243951.cif.'
_cod_database_code               7243941
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C18 N6 H12'
_reflns_odcompleteness_completeness 80.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     0.80
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C5 \\sim C4 \\sim C3 \\sim C2 \\sim C1 \\sim N11: within 1.7A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 1.7A
N12 \\sim C6 \\sim N13 \\sim C7: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
C8 \\sim C9 \\sim C10 \\sim N14: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
Uanis(C5) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(N11) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(N12) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(C4) \\sim Ueq,
Uanis(N14) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.025 and sigma for
terminal atoms of 0.5
Uanis(C8) \\sim Ueq: with sigma of 0.015 and sigma for terminal atoms of 0.3
3. Rigid body (RIGU) restrains
 C4, C3, C2, C1, N11, C5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N12, C6, N13, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C8, C9, C10, N14
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C1(H1), C2(H2), C9(H9), C10(H10)
4.b Fitted hexagon refined as free rotating group:
 C3(C4,C5,N11,C1,C2)
;
_shelx_res_checksum              36693
_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 2.351
_oxdiff_exptl_absorpt_empirical_full_min 0.227