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_1552090
_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         'O128 Si64'
_chemical_formula_sum            'O128 Si64'
_chemical_formula_weight         3845.38
_chemical_name_common            Mordenite
_chemical_name_systematic        Si-MOR
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c 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                   18.120
_cell_length_b                   20.000
_cell_length_c                   7.700
_cell_measurement_reflns_used    904
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      1.80
_cell_measurement_theta_min      0.072
_cell_volume                     2790.480
_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    'SHELXT-2014/5 (Sheldrick, 2013)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.570
_diffrn_measured_fraction_theta_max 0.549
_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  0.1014
_diffrn_reflns_av_unetI/netI     0.1620
_diffrn_reflns_Laue_measured_fraction_full 0.570
_diffrn_reflns_Laue_measured_fraction_max 0.549
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1941
_diffrn_reflns_point_group_measured_fraction_full 0.570
_diffrn_reflns_point_group_measured_fraction_max 0.549
_diffrn_reflns_theta_full        0.863
_diffrn_reflns_theta_max         0.911
_diffrn_reflns_theta_min         0.118
_diffrn_source                   'electron microscope'
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_density_diffrn    2.288
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             626
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       9988(43)
_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   2.159
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         904
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.159
_refine_ls_R_factor_all          0.3181
_refine_ls_R_factor_gt           0.2910
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_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          0.6105
_refine_ls_wR_factor_ref         0.6472
_reflns_Friedel_coverage         0.000
_reflns_number_gt                555
_reflns_number_total             904
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fc5033.cif
_cod_data_source_block           mordenite_mixed_phase
_cod_original_cell_volume        2790.5
_cod_database_code               1552090
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              94350
_shelx_hkl_checksum              79432