<i>Ab initio</i> structure determination of nanocrystals of organic pharmaceutical compounds by electron diffraction at room temperature using a Timepix quantum area direct electron detector
van Genderen, E.; Clabbers, M. T. B.; Das, P. P.; Stewart, A.; Nederlof, I.; Barentsen, K. C.; Portillo, Q.; Pannu, N. S.; Nicolopoulos, S.; Gruene, T.; Abrahams, J. P.; Acta Crystallographica Section A 72 (2016) 236–242; doi:10.1107/S2053273315022500

data_2311084
_publ_section_title
;
 <i>Ab initio</i> structure determination of nanocrystals of organic
 pharmaceutical compounds by electron diffraction at room temperature
 using a Timepix quantum area direct electron detector
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section A'
_journal_page_first              236
_journal_page_last               242
_journal_paper_doi               10.1107/S2053273315022500
_journal_volume                  72
_journal_year                    2016
_chemical_formula_sum            'C6 H5 N O2'
_chemical_formula_weight         123.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/8
_cell_angle_alpha                90
_cell_angle_beta                 114.45(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.41(3)
_cell_length_b                   11.692(2)
_cell_length_c                   7.377(11)
_cell_measurement_temperature    293(2)
_cell_volume                     582(3)
_computing_structure_refinement  'SHELXL-2014/8 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.392
_diffrn_measured_fraction_theta_max 0.390
_diffrn_measurement_device_type
;
 Philips EM30 LaB6 Electron Microscope with Timepix Detector
;
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.02508
_diffrn_reflns_av_R_equivalents  0.2703
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1337
_diffrn_reflns_theta_full        0.862
_diffrn_reflns_theta_max         0.953
_diffrn_reflns_theta_min         0.123
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       'data merged from 2 nanocrystals'
_exptl_crystal_F_000             256
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.816
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.216
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         552
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.216
_refine_ls_R_factor_all          0.4019
_refine_ls_R_factor_gt           0.3371
_refine_ls_shift/su_max          1.088
_refine_ls_shift/su_mean         0.028
_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          0.6328
_refine_ls_wR_factor_ref         0.6754
_reflns_number_gt                303
_reflns_number_total             552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            td5026sup1.cif
_cod_data_source_block           nicotinic_acid_2x-merged
_cod_depositor_comments
;
Adding full bibliography for 2311081--2311085.cif.

2017-03-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        581(2)
_cod_original_formula_sum        'C H0.83 N0.17 O0.33'
_cod_original_formula_units_Z    24
_cod_original_formula_weight     20.52
_cod_database_code               2311084
_cod_database_fobs_code          2311084
_shelx_hkl_checksum              81314
_shelx_res_checksum              29007