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_7243946
_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         'C12 H8 F3 N5 O3 S'
_chemical_formula_sum            'C12 H8 F3 N5 O3 S'
_chemical_formula_weight         359.29
_chemical_name_systematic
N-(2,6-difluorophenyl)-8-fluoro-5-methoxy-[1,2,4]triazolo[1,5-c]pyrimidine-2-sulfonamide
_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
_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                115.25(6)
_cell_angle_beta                 91.67(5)
_cell_angle_gamma                95.51(4)
_cell_formula_units_Z            2
_cell_length_a                   8.302(3)
_cell_length_b                   10.025(6)
_cell_length_c                   10.638(6)
_cell_measurement_reflns_used    314
_cell_measurement_temperature    293
_cell_measurement_theta_max      0.7568
_cell_measurement_theta_min      0.1105
_cell_volume                     794.7(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.18a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.18a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.18a (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    'SHELXD  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.15
_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 0.763
_diffrn_measured_fraction_theta_max 0.763
_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    -25.00  40.00   1.00    5.00    --    0.00   0.00   0.00   65
  2  \w    -30.00  40.00   1.00    5.00    --    0.00   0.00   0.00   70
  3  \w    -40.00  50.00   1.00    5.00    --    0.00   0.00   0.00   90
  4  \w    -10.00  40.00   1.00    5.00    --    0.00   0.00   0.00   50
  5  \w    -25.00  50.00   1.00    5.00    --    0.00   0.00   0.00   75
  6  \w    -25.00  50.00   1.00    5.00    --    0.00   0.00   0.00   75
  7  \w    -40.00  30.00   1.00    5.00    --    0.00   0.00   0.00   70
  8  \w    -45.00  30.00   1.00    5.00    --    0.00   0.00   0.00   75
  9  \w    -35.00  18.00   1.00    5.00    --    0.00   0.00   0.00   53
 10  \w    -50.00  15.00   1.00    5.00    --    0.00   0.00   0.00   65
;
_diffrn_measurement_device       'Electron diffractometer'
_diffrn_measurement_device_type  Synergy-ED
_diffrn_measurement_method       'continuous rotation'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0002675000
_diffrn_orient_matrix_UB_12      -0.0011818000
_diffrn_orient_matrix_UB_13      -0.0026164000
_diffrn_orient_matrix_UB_21      -0.0027171000
_diffrn_orient_matrix_UB_22      0.0009133000
_diffrn_orient_matrix_UB_23      0.0000343000
_diffrn_orient_matrix_UB_31      0.0013524000
_diffrn_orient_matrix_UB_32      0.0023546000
_diffrn_orient_matrix_UB_33      0.0000105000
_diffrn_radiation_probe          electron
_diffrn_radiation_type           '200 keV electrons'
_diffrn_radiation_wavelength     0.0251
_diffrn_reflns_av_R_equivalents  0.2081
_diffrn_reflns_av_unetI/netI     0.0960
_diffrn_reflns_Laue_measured_fraction_full 0.763
_diffrn_reflns_Laue_measured_fraction_max 0.763
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12066
_diffrn_reflns_point_group_measured_fraction_full 0.763
_diffrn_reflns_point_group_measured_fraction_max 0.763
_diffrn_reflns_theta_full        0.757
_diffrn_reflns_theta_max         0.757
_diffrn_reflns_theta_min         0.111
_diffrn_source                   'thermionic-emission electron gun'
_diffrn_source_type              LaB6
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.18a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       needle
_exptl_crystal_F_000             124
_exptl_crystal_recrystallization_method 'Re-crystallized on grid'
_exptl_crystal_size_max          0.0003
_exptl_crystal_size_mid          0.0003
_exptl_crystal_size_min          0.0003
_refine_diff_density_max         0.135
_refine_diff_density_min         -0.125
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       898(13)
_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   2.269
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         1482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.269
_refine_ls_R_factor_all          0.2143
_refine_ls_R_factor_gt           0.1602
_refine_ls_shift/su_max          0.009
_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          0.3630
_refine_ls_wR_factor_ref         0.3769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1077
_reflns_number_total             1482
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01172c1.cif
_cod_data_source_block           group2
_cod_depositor_comments
'Adding full bibliography for 7243939--7243951.cif.'
_cod_original_cell_volume        794.6(8)
_cod_database_code               7243946
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C12 H8 F3 N5 O3 S'
_reflns_odcompleteness_completeness 77.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     0.76
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N17(H17), C9(H9), C11(H11), C4(H4), C10(H10)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_shelx_res_checksum              81175
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.741
_oxdiff_exptl_absorpt_empirical_full_min 0.394