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_7247473
_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 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-07-20 deposited with the CCDC.	2023-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.710(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.4013(4)
_cell_length_b                   5.22360(10)
_cell_length_c                   22.4510(6)
_cell_measurement_reflns_used    7136
_cell_measurement_temperature    230.00(10)
_cell_measurement_theta_max      79.2670
_cell_measurement_theta_min      3.9610
_cell_volume                     1789.86(8)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      230.00(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 0.957
_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    -26.00  27.00   0.50    0.50    --  -49.12  19.00 -60.00  106
  2  \w   -120.00 -41.00   0.50    0.50    --  -49.12-178.00 -90.00  158
  3  \w    -26.00  27.00   0.50    0.50    --  -49.12  19.00 -30.00  106
  4  \w    -26.00  27.00   0.50    0.50    --  -49.12  19.00   0.00  106
  5  \w    -23.00 121.00   0.50    0.50    --   49.12   0.00 -90.00  288
  6  \w     62.00 120.00   0.50    0.50    --   49.12 178.00 -30.00  116
  7  \w    -43.00 -13.00   0.50    2.50    --  -88.50  38.00 -60.00   60
  8  \w    -43.00 -13.00   0.50    2.50    --  -88.50  38.00 -30.00   60
  9  \w    -43.00 -13.00   0.50    2.50    --  -88.50  38.00   0.00   60
 10  \w    -43.00 -13.00   0.50    2.50    --  -88.50  38.00  30.00   60
 11  \w    -43.00 -13.00   0.50    2.50    --  -88.50  38.00 150.00   60
 12  \w   -160.00 -73.00   0.50    2.50    --  -88.50 -57.00-150.00  174
 13  \w     38.00  66.00   0.50    2.50    --  110.00 -57.00 -90.00   56
 14  \w     97.00 178.00   0.50    2.50    --  110.00  19.00 150.00  162
 15  \w     38.00  66.00   0.50    2.50    --  110.00 -57.00 -30.00   56
 16  \w     98.00 178.00   0.50    2.50    --  110.00  38.00  30.00  160
 17  \w     38.00  66.00   0.50    2.50    --  110.00 -57.00 150.00   56
 18  \w     38.00  66.00   0.50    2.50    --  110.00 -57.00 -60.00   56
 19  \w     45.00 105.00   0.50    2.50    --  110.00 -77.00  90.00  120
 20  \w     38.00  66.00   0.50    2.50    --  110.00 -57.00   0.00   56
 21  \w     97.00 178.00   0.50    2.50    --  110.00  19.00  90.00  162
 22  \w     38.00  66.00   0.50    2.50    --  110.00 -57.00 120.00   56
 23  \w   -114.00 -25.00   0.50    0.50    --  -49.12 -77.00 -30.00  178
 24  \w     26.00 114.00   0.50    0.50    --   49.12  77.00-120.00  176
 25  \w     26.00 114.00   0.50    0.50    --   49.12  77.00  60.00  176
 26  \w     62.00 120.00   0.50    0.50    --   49.12 178.00-150.00  116
 27  \w     37.00 125.00   0.50    0.50    --   49.12  19.00  30.00  176
;
_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      0.0724311000
_diffrn_orient_matrix_UB_12      0.1808341000
_diffrn_orient_matrix_UB_13      -0.0159702000
_diffrn_orient_matrix_UB_21      0.0516617000
_diffrn_orient_matrix_UB_22      -0.0422956000
_diffrn_orient_matrix_UB_23      0.0628801000
_diffrn_orient_matrix_UB_31      0.0477309000
_diffrn_orient_matrix_UB_32      -0.2290427000
_diffrn_orient_matrix_UB_33      -0.0241911000
_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  0.0352
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            18393
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.551
_diffrn_reflns_theta_min         3.974
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.816
_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    1.322
_exptl_crystal_description       plate
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.031
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         3731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0766P)^2^+0.1768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1620
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2638
_reflns_number_total             3731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00940h2.cif
_cod_data_source_block           tp_bacidup_04_230_00
_cod_depositor_comments
'Adding full bibliography for 7247467--7247477.cif.'
_cod_database_code               7247473
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C10 H10 O3'
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.799
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
2.a Idealised tetrahedral OH refined as rotating group:
 O2(H2), O2A(H2AA)
;
_shelx_res_checksum              8460
_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 1.878
_oxdiff_exptl_absorpt_empirical_full_min 0.498