Electron diffraction determines molecular absolute configuration in a pharmaceutical nanocrystal
Brázda, Petr; Palatinus, Lukáš; Babor, Martin; Science 364 (2019) 667–669; doi:10.1126/science.aaw2560

data_3000217
_publ_section_title
;
 Electron diffraction determines molecular absolute configuration in a
 pharmaceutical nanocrystal
;
_journal_issue                   6441
_journal_name_full               Science
_journal_page_first              667
_journal_page_last               669
_journal_paper_doi               10.1126/science.aaw2560
_journal_volume                  364
_journal_year                    2019
_chemical_formula_moiety         'C22 H29 F1 N3 O9 P1, C5 H9 N1 O2'
_chemical_formula_sum            'C27 H38 F N4 O11 P'
_chemical_formula_weight         644.58
_chemical_name_common            'Sofosbuvir, L-proline'
_space_group_IT_number           19
_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                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   5.34
_cell_length_b                   19.53
_cell_length_c                   29.98
_cell_measurement_temperature    100
_cell_volume                     3126.620
_computing_cell_refinement
;
Jana2006 (Petricek et al., 2014).
;
_computing_data_collection
;
PETS (Palatinus, L., 2011).
;
_computing_data_reduction
;
PETS (Palatinus, L., 2011).
;
_computing_molecular_graphics
;
Diamond version 3 (Brandenburg, K., 2005).
;
_computing_structure_refinement
;
Jana2006 (Petricek et al., 2014).
Dynamical refinement (Palatinus, L. <i>et al.<i> 2015).
;
_computing_structure_solution
;
SIR2011 (Brla M.C. et al.).
;
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD camera Olympus SIS Veleta'
_diffrn_detector_area_resol_mean 2048.2048
_diffrn_measurement_device       'Transmission electron microscope'
_diffrn_measurement_device_type  'Philips CM120'
_diffrn_measurement_method       PEDT
_diffrn_measurement_specimen_support 'Cu grid with carbon foil'
_diffrn_radiation_probe          electron
_diffrn_radiation_source         'Lanthanum hexaboride cathode'
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.0335
_diffrn_reflns_number            48871
_diffrn_reflns_reduction_process
'data integration using rocking curve profile with PETS'
_diffrn_source                   electron
_diffrn_source_voltage           120
_exptl_crystal_colour            none
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
ribbon-shaped crystal on carbon film of Cu TEM grid
;
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.001
_exptl_crystal_size_mid          0.0005
_exptl_crystal_size_min          0.00007
_refine_ls_abs_structure_details
'  1132 of Friedel pairs used in the refinement'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    3.01
_refine_ls_goodness_of_fit_ref   2.40
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_constraints    132
_refine_ls_number_parameters     266
_refine_ls_number_reflns         5071
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1623
_refine_ls_R_factor_gt           0.0986
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/(\s^2^(F)+0.0001F^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                2985
_reflns_number_total             5071
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            SF_L-proline_normal_final_check.cif
_cod_data_source_block           I
_cod_depositor_comments
;By accicent the originally deposited structure had wrong absolute
 structure. The updated cif corrects this error.

 Releasing structure 3000217 into public domain as published material.
;
_cod_original_cell_volume        3127
_cod_original_formula_sum        'C27 H38 F1 N4 O11 P1'
_cod_database_code               3000217
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n