Melting pseudosymmetry and thermal expansion in 3-benzoylpropionic acid
Poręba, Tomasz; Świątkowski, Marcin; Confalonieri, Giorgia; CrystEngComm 25 (2023) 5932–5941; doi:10.1039/D3CE00940H

data_7247476
_publ_section_title
;
 Melting pseudosymmetry and thermal expansion in 3-benzoylpropionic acid
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              5932
_journal_page_last               5941
_journal_paper_doi               10.1039/D3CE00940H
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C10 H10 O3'
_chemical_formula_sum            'C10 H10 O3'
_chemical_formula_weight         178.18
_chemical_name_common            '3-benzoylpropionic acid'
_chemical_name_systematic        '3-benzoylpropionic acid'
_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   difmap
_audit_creation_date             2023-06-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-20 deposited with the CCDC.	2023-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.423(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7932(5)
_cell_length_b                   5.23468(18)
_cell_length_c                   14.4811(6)
_cell_measurement_reflns_used    4573
_cell_measurement_temperature    269.99(10)
_cell_measurement_theta_max      75.5300
_cell_measurement_theta_min      3.9300
_cell_volume                     902.77(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.68a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.68a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.68a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      269.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.905
_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     42.00  83.00   0.50    1.50    --  110.00 -68.00 138.00   82
  2  \w     45.00 105.00   0.50    1.50    --  110.00 -77.00  60.00  120
  3  \w     38.00  66.00   0.50    1.50    --  110.00 -57.00 -30.00   56
  4  \w     38.00  66.00   0.50    1.50    --  110.00 -57.00 -60.00   56
  5  \w     38.00  66.00   0.50    1.50    --  110.00 -57.00 -90.00   56
  6  \w     38.00  66.00   0.50    1.50    --  110.00 -57.00-180.00   56
  7  \w     38.00  66.00   0.50    1.50    --  110.00 -57.00 120.00   56
  8  \w     26.00 114.00   0.50    0.30    --   49.12  77.00  90.00  176
  9  \w     26.00 114.00   0.50    0.30    --   49.12  77.00 -30.00  176
 10  \w     62.00 120.00   0.50    0.30    --   49.12 178.00-120.00  116
 11  \w     26.00 114.00   0.50    0.30    --   49.12  77.00-150.00  176
 12  \w    -26.00  27.00   0.50    0.30    --  -49.12  19.00 -60.00  106
 13  \w     60.00 122.00   0.50    0.30    --   49.12-178.00   0.00  124
 14  \w    -26.00  27.00   0.50    0.30    --  -49.12  19.00   0.00  106
 15  \w    -26.00  27.00   0.50    0.30    --  -49.12  19.00  30.00  106
 16  \w    -26.00  27.00   0.50    0.30    --  -49.12  19.00 150.00  106
 17  \w    -66.00 -17.00   0.50    1.50    --  -88.50  57.00  60.00   98
 18  \w    -43.00 -13.00   0.50    1.50    --  -88.50  38.00  90.00   60
 19  \w    -43.00 -13.00   0.50    1.50    --  -88.50  38.00  30.00   60
 20  \w    -43.00 -13.00   0.50    1.50    --  -88.50  38.00 150.00   60
 21  \w    -43.00 -13.00   0.50    1.50    --  -88.50  38.00   0.00   60
 22  \w    -43.00 -13.00   0.50    1.50    --  -88.50  38.00-120.00   60
 23  \w    -43.00 -13.00   0.50    1.50    --  -88.50  38.00-180.00   60
 24  \w    -43.00 -13.00   0.50    1.50    --  -88.50  38.00-150.00   60
 25  \w    -43.00 -13.00   0.50    1.50    --  -88.50  38.00 -90.00   60
 26  \w   -164.00 -75.00   0.50    1.50    --  -88.50 -19.00   0.00  178
 27  \w   -160.00-127.00   0.50    1.50    --  -88.50 -57.00 120.00   66
 28  \w   -120.00 -41.00   0.50    0.30    --  -49.12-178.00 -60.00  158
 29  \w   -157.00 -85.00   0.50    1.50    --  -88.50 -99.00 -30.00  144
 30  \w   -154.00 -65.00   0.50    1.50    --  -88.50 -77.00 -60.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0104505000
_diffrn_orient_matrix_UB_12      -0.1796341000
_diffrn_orient_matrix_UB_13      0.0804406000
_diffrn_orient_matrix_UB_21      0.1271114000
_diffrn_orient_matrix_UB_22      -0.0535262000
_diffrn_orient_matrix_UB_23      0.0367321000
_diffrn_orient_matrix_UB_31      0.0216987000
_diffrn_orient_matrix_UB_32      0.2269176000
_diffrn_orient_matrix_UB_33      0.0723493000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9246
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.723
_diffrn_reflns_theta_min         3.955
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.949
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.68a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.311
_exptl_crystal_description       plate
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.288
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.168
_refine_diff_density_min         -0.167
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         1785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0610P)^2^+0.0982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1232
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1418
_reflns_number_total             1785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00940h2.cif
_cod_data_source_block           tp_bacidup_10_270_00
_cod_depositor_comments
'Adding full bibliography for 7247467--7247477.cif.'
_cod_original_cell_volume        902.77(6)
_cod_database_code               7247476
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C10 H10 O3'
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.798
_olex2_refinement_description
;
;
_shelx_res_checksum              10739
_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 4.573
_oxdiff_exptl_absorpt_empirical_full_min 0.389