Theoretically derived thermodynamic properties can be improved by the refinement of low-frequency modes against X-ray diffraction data.
Hoser, Anna A.; Sztylko, Marcin; Trzybiński, Damian; Madsen, Anders Ø; Chemical communications (Cambridge, England) 57 (2021) 9370–9373; doi:10.1039/d1cc02608a

data_7128792
_publ_section_title
;
 Theoretically derived thermodynamic properties can be improved by the
 refinement of low-frequency modes against X-ray diffraction data.
;
_journal_issue                   74
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9370
_journal_page_last               9373
_journal_paper_doi               10.1039/d1cc02608a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C2 H5 N O2'
_chemical_formula_sum            'C2 H5 N O2'
_chemical_formula_weight         75.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-03
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;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-13 deposited with the CCDC.	2021-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.983(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.0867(2)
_cell_length_b                   11.7982(4)
_cell_length_c                   5.4598(2)
_cell_measurement_reflns_used    2421
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.1190
_cell_measurement_theta_min      3.4450
_cell_volume                     303.84(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~1~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0026
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -103.00 -49.00   1.00    3.00    --  -29.20-160.00-150.00   54
  2  \w   -103.00 -49.00   1.00    3.00    --  -29.20-160.00 150.00   54
  3  \w    -61.00  44.00   1.00    3.00    --  -29.20  37.00-150.00  105
  4  \w   -100.00  -6.00   1.00    3.00    --  -29.20 -57.00  60.00   94
  5  \w   -103.00 -49.00   1.00    3.00    --  -29.20-160.00 -60.00   54
  6  \w   -100.00  -6.00   1.00    3.00    --  -29.20 -57.00-150.00   94
  7  \w   -100.00  -6.00   1.00    3.00    --  -29.20 -57.00 -60.00   94
  8  \w   -100.00  -6.00   1.00    3.00    --  -29.20 -57.00 120.00   94
  9  \w   -109.00 -81.00   1.00    3.00    --  -29.20 160.00   0.00   28
 10  \w    -35.00  -6.00   1.00    3.00    --   29.36 132.00 -14.89   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1398664000
_diffrn_orient_matrix_UB_12      0.0094233000
_diffrn_orient_matrix_UB_13      0.0920511000
_diffrn_orient_matrix_UB_21      0.0331034000
_diffrn_orient_matrix_UB_22      0.0292657000
_diffrn_orient_matrix_UB_23      -0.0983003000
_diffrn_orient_matrix_UB_31      -0.0442156000
_diffrn_orient_matrix_UB_32      0.0516392000
_diffrn_orient_matrix_UB_33      0.0388900000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4778
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.505
_diffrn_reflns_theta_min         3.454
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_description       block
_exptl_crystal_F_000             160
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         932
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+0.1369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0841
_reflns_Friedel_coverage         0.000
_reflns_number_gt                809
_reflns_number_total             932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02608a2.cif
_cod_data_source_block           2015_09_09_dt_alpha-gly_d
_cod_depositor_comments
'Adding full bibliography for 7128792--7128793.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7128792
_shelx_shelxl_version_number     2016/4
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All O(H,H,H) groups
2. Restrained distances
 N1-H1B
 0.87 with sigma of 0.01
 N1-H1A
 0.87 with sigma of 0.01
 N1-H1C
 0.87 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C2(H2B,H2A)
;
_shelx_res_checksum              59376
_shelx_hkl_checksum              15088
_olex2_date_sample_data_collection 2015-09-09
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.527
_oxdiff_exptl_absorpt_empirical_full_min 0.774