On the importance of low-frequency modes in predicting pressure-induced phase transitions.
Hoser, Anna; Zwolenik, Aleksandra; Makal, Anna; Physical chemistry chemical physics : PCCP 26 (2024) 20745–20749; doi:10.1039/d4cp02368d

data_7249112
_publ_section_title
;
 On the importance of low-frequency modes in predicting pressure-induced
 phase transitions.
;
_journal_issue                   31
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              20745
_journal_page_last               20749
_journal_paper_doi               10.1039/d4cp02368d
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         '2(C10 H7 O)'
_chemical_formula_sum            'C20 H14 O2'
_chemical_formula_weight         286.31
_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   geom
_audit_creation_date             2024-01-25
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.11.24 svn.r209d9fb for OlexSys, GUI svn.r6869)
;
_audit_update_record
;
2024-02-13 deposited with the CCDC.	2024-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.75(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.017(3)
_cell_length_b                   23.00(3)
_cell_length_c                   7.369(3)
_cell_measurement_reflns_used    688
_cell_measurement_temperature    287(7)
_cell_measurement_theta_max      31.4710
_cell_measurement_theta_min      2.6420
_cell_volume                     1351.9(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_pressure         510000
_diffrn_ambient_temperature      287.15
_diffrn_crystal_treatment
'pressurized slowly/rapidly in paratone oil as a hydrostatic medium'
_diffrn_detector_area_resol_mean 5.2195
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.566
_diffrn_measured_fraction_theta_max 0.389
_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    -14.00  41.00   1.00   60.00    --   18.10  26.00 172.00   55
  2  \w    -15.00  21.00   1.00   60.00    --   18.10  81.00 -29.00   36
  3  \w    -14.00  48.00   1.00   60.00    --   18.10 -97.00  35.00   62
  4  \w    -19.00   9.00   1.00   60.00    --   18.10 -53.00  17.00   28
  5  \w     55.00  95.00   1.00   60.00    --   18.10-178.00  90.00   40
  6  \w    -43.00   6.00   1.00   60.00    --   18.10  13.00  -3.00   49
  7  \w    -75.00 -49.00   1.00   60.00    --  -19.97 134.00 -57.00   26
  8  \w    -20.00   5.00   1.00   60.00    --  -19.97 -39.00-167.00   25
  9  \w      8.00  33.00   1.00   60.00    --  -19.97-134.00-123.00   25
 10  \w    -15.00   8.00   1.00   60.00    --  -19.97 -57.00  30.00   23
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support
'Diamond Anvil Cell, effective opening angle of 40 deg.'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_unetI/netI     0.2123
_diffrn_reflns_Laue_measured_fraction_full 0.566
_diffrn_reflns_Laue_measured_fraction_max 0.389
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4593
_diffrn_reflns_point_group_measured_fraction_full 0.566
_diffrn_reflns_point_group_measured_fraction_max 0.389
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.729
_diffrn_reflns_theta_min         2.703
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43d (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       plate
_exptl_crystal_F_000             600
_exptl_crystal_preparation
'Mounted in a Diamond-Anvil Cell using paratone oil as pressure medium.'
_exptl_crystal_pressure_history  'Pressurized to 0.51 GPa.'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.166
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         1938
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.3215
_refine_ls_R_factor_gt           0.1480
_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^)+(0.0189P)^2^+2.1477P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1628
_refine_ls_wR_factor_ref         0.2140
_reflns_Friedel_coverage         0.000
_reflns_number_gt                812
_reflns_number_total             1938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cp02368d2.cif
_cod_data_source_block           2papb_0p5gpa
_cod_depositor_comments
'Adding full bibliography for 7249110--7249118.cif.'
_cod_original_cell_volume        1352.1(18)
_cod_database_code               7249112
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C1B, C2B, C3B, C4B, C5B, C6B, C7B, C8B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C5A(H5A), C6A(H6A), C7A(H7A), C1B(H1B), C5B(H5B), C6B(H6B), C7B(H7B)
3.b Idealised Me refined as rotating group:
 C10A(H10A,H10B,H10C), C10B(H10D,H10E,H10F)
;
_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
;