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_1552093
_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         'C192 O96.16 Ti16 Zr4'
_chemical_formula_sum            'C192 O96.16 Ti16 Zr4'
_chemical_formula_weight         4975.28
_chemical_name_common            PCN-416
_chemical_name_systematic        PCN-416
_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_Hall           'I -4 2'
_space_group_name_H-M_alt        'I -4 2 m'
_symmetry_space_group_name_Hall  'I -4 2'
_symmetry_space_group_name_H-M   'I -4 2 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                   16.5(4)
_cell_length_b                   16.5(4)
_cell_length_c                   29.8(8)
_cell_measurement_reflns_used    2825
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      1.80
_cell_measurement_theta_min      0.072
_cell_volume                     8113(4)
_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 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.2295
_diffrn_reflns_av_unetI/netI     0.2829
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            11248
_diffrn_reflns_point_group_measured_fraction_full 0.923
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        0.797
_diffrn_reflns_theta_max         0.797
_diffrn_reflns_theta_min         0.085
_diffrn_source                   'electron microscope'
_exptl_absorpt_coefficient_mu    0.000
_exptl_crystal_density_diffrn    1.020
_exptl_crystal_description       nano-crystals
_exptl_crystal_F_000             1010
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 All f" are zero, so absolute structure could not be determined
;
_refine_ls_extinction_coef       147(52)
_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   1.301
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2825
_refine_ls_number_restraints     377
_refine_ls_restrained_S_all      1.258
_refine_ls_R_factor_all          0.2785
_refine_ls_R_factor_gt           0.2163
_refine_ls_shift/su_max          0.002
_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^+1.0000sin\q/\l] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4738
_refine_ls_wR_factor_ref         0.5351
_reflns_Friedel_coverage         0.734
_reflns_Friedel_fraction_full    0.871
_reflns_Friedel_fraction_max     0.871
_reflns_number_gt                1254
_reflns_number_total             2825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fc5033.cif
_cod_data_source_block           PCN416
_cod_original_cell_volume        8086(480)
_cod_database_code               1552093
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              54384
_shelx_hkl_checksum              10101