Automated serial rotation electron diffraction combined with cluster analysis: an efficient multi-crystal workflow for structure determination
Wang, Bin; Zou, Xiaodong; Smeets, Stef; IUCrJ 6 (2019) –; doi:10.1107/S2052252519007681

data_1552091
_publ_section_title
;
 Automated serial rotation electron diffraction combined with cluster
 analysis: an efficient multi-crystal workflow for structure determination
;
_journal_issue                   5
_journal_name_full               IUCrJ
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052252519007681
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         'O5280 Si2640'
_chemical_formula_sum            'O5280 Si2640'
_chemical_formula_weight         158620.44
_chemical_name_common            PST-20
_chemical_name_systematic        PST-20
_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_Hall           '-I 4 2 3'
_space_group_name_H-M_alt        'I m -3 m'
_symmetry_space_group_name_Hall  '-I 4 2 3'
_symmetry_space_group_name_H-M   'I m -3 m'
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   55.070
_cell_length_b                   55.070
_cell_length_c                   55.070
_cell_measurement_reflns_used    2647
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0.963
_cell_measurement_theta_min      0.072
_cell_volume                     167011.059
_computing_cell_refinement       'XDS-20180126 (Kabsch, 2018)'
_computing_data_collection       'Instamatic-1.0.0 (Smeets et al., 2018)'
_computing_data_reduction        'XDS-20180126 (Kabsch, 2018)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'FOCUS (Grosse-Kunstleve et al., 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'JEOL JEM-2100 LaB6'
_diffrn_measurement_method       'Continuous rotation electron diffraction'
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.0251
_diffrn_reflns_av_R_equivalents  0.3801
_diffrn_reflns_av_unetI/netI     0.1378
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            92346
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        0.490
_diffrn_reflns_theta_max         0.490
_diffrn_reflns_theta_min         0.041
_diffrn_source                   'electron microscope'
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       cubes
_exptl_crystal_F_000             25829
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.17(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   3.224
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         2647
_refine_ls_number_restraints     292
_refine_ls_restrained_S_all      3.092
_refine_ls_R_factor_all          0.5294
_refine_ls_R_factor_gt           0.4900
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.8459
_refine_ls_wR_factor_ref         0.8583
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1179
_reflns_number_total             2647
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fc5033.cif
_cod_data_source_block           pst20_mixed_phase
_cod_original_cell_volume        167011.0
_cod_database_code               1552091
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              80416
_shelx_hkl_checksum              74761