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_7243951
_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         'C42 H28 Fe N10'
_chemical_formula_sum            'C42 H28 Fe N10'
_chemical_formula_weight         728.59
_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   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                 111.6(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.25(12)
_cell_length_b                   19.99(19)
_cell_length_c                   9.66(10)
_cell_measurement_reflns_used    2667
_cell_measurement_temperature    293
_cell_measurement_theta_max      0.8730
_cell_measurement_theta_min      0.1160
_cell_volume                     1661(3)
_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 0.953
_diffrn_measured_fraction_theta_max 0.953
_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  35.00   1.00    4.00    --    0.00   0.00   0.00   75
  2  \w    -25.00  50.00   1.00    4.00    --    0.00   0.00   0.00   75
  3  \w    -20.00  55.00   1.00    4.00    --    0.00   0.00   0.00   75
  4  \w    -30.00  40.00   1.00    4.00    --    0.00   0.00   0.00   70
;
_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      -0.0000293000
_diffrn_orient_matrix_UB_12      -0.0012391000
_diffrn_orient_matrix_UB_13      -0.0004171000
_diffrn_orient_matrix_UB_21      -0.0013820000
_diffrn_orient_matrix_UB_22      -0.0001713000
_diffrn_orient_matrix_UB_23      0.0017748000
_diffrn_orient_matrix_UB_31      -0.0025691000
_diffrn_orient_matrix_UB_32      0.0001064000
_diffrn_orient_matrix_UB_33      -0.0021157000
_diffrn_radiation_probe          electron
_diffrn_radiation_type           '200 keV electrons'
_diffrn_radiation_wavelength     0.0251
_diffrn_reflns_av_R_equivalents  0.1937
_diffrn_reflns_av_unetI/netI     0.0997
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13977
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        0.799
_diffrn_reflns_theta_max         0.799
_diffrn_reflns_theta_min         0.108
_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  0.05186
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.13a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       block
_exptl_crystal_F_000             299
_exptl_crystal_size_max          0.0004
_exptl_crystal_size_mid          0.0002
_exptl_crystal_size_min          0.0002
_refine_diff_density_max         0.161
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       1502(42)
_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   1.276
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         2281
_refine_ls_number_restraints     225
_refine_ls_restrained_S_all      1.218
_refine_ls_R_factor_all          0.1773
_refine_ls_R_factor_gt           0.1659
_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^)+(0.0817P)^2^+1.9940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3547
_refine_ls_wR_factor_ref         0.3604
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2016
_reflns_number_total             2281
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01172c1.cif
_cod_data_source_block           15_4_11_13
_cod_depositor_comments
'Adding full bibliography for 7243939--7243951.cif.'
_cod_original_cell_volume        1662(33)
_cod_database_code               7243951
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C32 H18 N8 Fe'
_reflns_odcompleteness_completeness 97.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     0.80
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
C4 \\sim C3 \\sim C2 \\sim C1 \\sim C6 \\sim C5: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
N24 \\sim C8 \\sim N23 \\sim C7 \\sim N22 \\sim Fe27: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 1.7A
C14 \\sim C13 \\sim C12 \\sim C11 \\sim C10 \\sim C15: within 1.7A with sigma
of 0.03 and sigma for terminal atoms of 0.06 within 1.7A
3. Rigid body (RIGU) restrains
 C8, N23, C7, N22, Fe27, N24
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C4, C3, C2, C1, C6, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C14, C13, C12, C11, C10, C15
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
 C16, N26, C19, C18, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 N23(H23), C16(H16), C20(H20), C12(H12), C13(H13), C4(H4), C15(H15), C17(H17),
 C1(H1), C14(H14), C2(H2), C3(H3), C19(H19), C18(H18)
;
_shelx_res_checksum              34756
_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 2.487
_oxdiff_exptl_absorpt_empirical_full_min 0.163