Optimal estimated standard uncertainties of reflection intensities for kinematical refinement from 3D electron diffraction data
Khouchen, Malak; Klar, Paul Benjamin; Chintakindi, Hrushikesh; Suresh, Ashwin; Palatinus, Lukas; Acta Crystallographica Section A Foundations and Advances 79 (2023) 427–439; doi:10.1107/S2053273323005053

data_2312294
_publ_section_title
;
 Optimal estimated standard uncertainties of reflection intensities for
 kinematical refinement from 3D electron diffraction data
;
_journal_coeditor_code           PL5027
_journal_issue                   5
_journal_name_full
'Acta Crystallographica Section A Foundations and Advances'
_journal_page_first              427
_journal_page_last               439
_journal_paper_doi               10.1107/S2053273323005053
_journal_volume                  79
_journal_year                    2023
_chemical_absolute_configuration rm
_chemical_formula_sum            'C3 H7 N O2'
_chemical_formula_weight         89.1
_chemical_name_common            DL-alanine
_chemical_name_systematic        DL-alanine
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.7733(11)
_cell_length_b                   5.9524(12)
_cell_length_c                   12.2465(2)
_cell_measurement_reflns_used    3422
_cell_measurement_temperature    100
_cell_measurement_theta_max      1.44
_cell_measurement_theta_min      0.12
_cell_volume                     420.85(12)
_computing_cell_refinement       PETS2
_computing_data_collection       'self-written scripts, OLYMPUS iTEM'
_computing_data_reduction        PETS2
_computing_molecular_graphics    'VESTA 3'
_computing_structure_refinement  Jana2020
_computing_structure_solution    superflip
_diffrn_ambient_temperature      100
_diffrn_detector                 ASI
_diffrn_measured_fraction_theta_full 0.84
_diffrn_measured_fraction_theta_max 0.55
_diffrn_measurement_device       'TEM FEI Tecnai G2 20'
_diffrn_measurement_method       'continuous-rotation 3D ED'
_diffrn_measurement_specimen_support 'holey carbon grid'
_diffrn_radiation_probe          electron
_diffrn_radiation_source         'Lab6 cathode'
_diffrn_radiation_type           'electrons 200 keV'
_diffrn_radiation_wavelength     0.0251
_diffrn_reflns_av_R_equivalents  0.111
_diffrn_reflns_av_unetI/netI     0.1238
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            3422
_diffrn_reflns_theta_full        1.09
_diffrn_reflns_theta_max         1.44
_diffrn_reflns_theta_min         0.12
_exptl_crystal_density_diffrn    1.4061
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             69.628
_refine_diff_density_max         0.23
_refine_diff_density_min         -0.18
_refine_ls_extinction_coef       30(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick, 2015)'
_refine_ls_goodness_of_fit_gt    2.6013
_refine_ls_goodness_of_fit_ref   2.5650
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_constraints    63
_refine_ls_number_parameters     56
_refine_ls_number_reflns         1127
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1473
_refine_ls_R_factor_gt           0.1444
_refine_ls_shift/su_max          0.0171
_refine_ls_shift/su_mean         0.0041
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.02P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.3517
_refine_ls_wR_factor_ref         0.3551
_reflns_number_gt                1072
_reflns_number_total             1127
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            pl5027.cif
_cod_data_source_block           L-alanine_model3
_cod_original_cell_volume        420.85(14)
_cod_original_sg_symbol_Hall     'P 2xab;2ybc;2zac'
_cod_database_code               2312294