Structural transformations and stability of benzo[a]pyrene under high pressure.
Zhou, Wenju; Aslandukov, Andrey; Minchenkova, Anastasiia; Hanfland, Michael; Dubrovinsky, Leonid; Dubrovinskaia, Natalia; IUCrJ 12 (2025) –; doi:10.1107/S2052252524010455

data_1573200
_publ_section_title
;
 Structural transformations and stability of benzo[a]pyrene under high
 pressure.
;
_journal_issue                   1
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252524010455
_journal_volume                  12
_journal_year                    2025
_chemical_formula_moiety         'C20 H12'
_chemical_formula_sum            'C20 H12'
_chemical_formula_weight         252.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-08-18
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                91.56(3)
_cell_angle_beta                 89.92(3)
_cell_angle_gamma                95.171(13)
_cell_formula_units_Z            4
_cell_length_a                   3.1077(4)
_cell_length_b                   11.995(2)
_cell_length_c                   20.571(8)
_cell_measurement_reflns_used    482
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.0950
_cell_measurement_theta_min      3.8450
_cell_volume                     763.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 13.3333
_diffrn_measured_fraction_theta_full 0.206
_diffrn_measured_fraction_theta_max 0.203
_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    -32.50  21.00   0.50    1.00    --    0.00   0.00   0.00  107
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.410
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.206
_diffrn_reflns_Laue_measured_fraction_max 0.203
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            988
_diffrn_reflns_point_group_measured_fraction_full 0.206
_diffrn_reflns_point_group_measured_fraction_max 0.203
_diffrn_reflns_theta_full        14.241
_diffrn_reflns_theta_max         15.861
_diffrn_reflns_theta_min         3.798
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.057
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.04366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.195
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.023
_exptl_crystal_size_mid          0.021
_exptl_crystal_size_min          0.018
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.677
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         764
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.476
_refine_ls_R_factor_all          0.1824
_refine_ls_R_factor_gt           0.1427
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_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          0.3240
_refine_ls_wR_factor_ref         0.3640
_reflns_Friedel_coverage         0.000
_reflns_number_gt                431
_reflns_number_total             764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lq5058.cif
_cod_data_source_block           benzoapyrene_27.9GPa
_cod_database_code               1573200
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C33) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C7) \\sim Ueq,
Uanis(C23) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C59)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C45) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C55)
\\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C77) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.02
Uanis(C43) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C61) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C35) \\sim Ueq,
Uanis(C21) \\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C21) \\sim Ueq, Uanis(C71) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C27(H27), C29(H29), C31(H31), C33(H33), C35(H35), C37(H37),
 C39(H39), C41(H41), C43(H43), C49(H49), C51(H51), C57(H57), C59(H59), C61(H61),
  C63(H63), C65(H65), C67(H67), C69(H69), C71(H71), C73(H73), C75(H75),
 C77(H77), C79(H79)
;
_shelx_res_checksum              2558
_shelx_hkl_checksum              33464
_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
;