Evolution of structure and spectroscopic properties of a new 1,3-diacetylpyrene polymorph with temperature and pressure.
Zwolenik, A.; Tchoń, D; Makal, A.; IUCrJ 11 (2024) –; doi:10.1107/S2052252524003634

data_1571597
_publ_section_title
;
 Evolution of structure and spectroscopic properties of a new
 1,3-diacetylpyrene polymorph with temperature and pressure.
;
_journal_coeditor_code           YC5047
_journal_issue                   4
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252524003634
_journal_volume                  11
_journal_year                    2024
_chemical_formula_moiety         'C20 H14 O2'
_chemical_formula_sum            'C20 H14 O2'
_chemical_formula_weight         286.333
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     direct
_audit_creation_date             2023-01-23
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.4944(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.15110(13)
_cell_length_b                   10.90793(19)
_cell_length_c                   17.7744(3)
_cell_measurement_reflns_used    19785
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      34.4320
_cell_measurement_theta_min      3.3090
_cell_volume                     1353.63(4)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.9493
_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    -52.00  43.00   0.50   80.00    --   30.50 -49.00  90.00  190
  2  \w     -9.00 112.00   0.50   80.00    --   30.50  49.00-122.00  242
  3  \w    -75.00 -39.00   0.50   80.00    --  -30.81 -49.00  90.00   72
  4  \w    -12.00 116.00   0.50   80.00    --   30.50  77.00  90.00  256
  5  \w     56.00 114.00   0.50   80.00    --   30.50 178.00  90.00  116
  6  \w    -49.00 -23.00   0.50   80.00    --   30.50  19.00-150.00   52
  7  \w    -12.00  78.00   0.50   80.00    --   30.50  77.00 -60.00  180
  8  \w     -4.00 117.00   0.50   80.00    --   30.50  19.00-150.00  242
  9  \w     -2.00 110.00   0.50   80.00    --   30.50  57.00  60.00  224
 10  \w   -126.00 -61.00   0.50   80.00    --  -30.81 178.00 -90.00  130
 11  \w   -124.00 -63.00   0.50   80.00    --  -30.81-178.00-180.00  122
 12  \w   -116.00   8.00   0.50   80.00    --  -30.81 -38.00 -90.00  248
 13  \w   -118.00  54.00   0.50   80.00    --  -30.81  19.00-150.00  344
 14  \w   -126.00 -73.00   0.50   80.00    --  -30.81-178.00  30.00  106
 15  \w    -22.00  16.00   0.50   80.00    --  -30.81 -99.00 150.00   76
 16  \w    -38.00  43.00   0.50   80.00    --  -30.81  49.00-122.00  162
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0575942284
_diffrn_orient_matrix_UB_12      -0.0442814338
_diffrn_orient_matrix_UB_13      0.0234894896
_diffrn_orient_matrix_UB_21      0.0836230409
_diffrn_orient_matrix_UB_22      0.0287614565
_diffrn_orient_matrix_UB_23      -0.0069440485
_diffrn_orient_matrix_UB_31      0.0037924276
_diffrn_orient_matrix_UB_32      0.0379375689
_diffrn_orient_matrix_UB_33      0.0327143467
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.9984
_diffrn_reflns_Laue_measured_fraction_max 0.9493
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            48392
_diffrn_reflns_point_group_measured_fraction_full 0.9984
_diffrn_reflns_point_group_measured_fraction_max 0.9493
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         34.57
_diffrn_reflns_theta_min         3.33
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43d (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
   a multifaceted crystal model
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    1.405
_exptl_crystal_description       irregular
_exptl_crystal_F_000             600.369
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.2407
_refine_diff_density_min         -0.2340
_refine_diff_density_rms         0.0557
_refine_ls_d_res_high            0.6263
_refine_ls_d_res_low             6.1250
_refine_ls_goodness_of_fit_ref   1.0435
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0435
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0120P)^2^+0.0116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0391
_refine_ls_wR_factor_ref         0.0421
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -11
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                4111
_reflns_number_total             5486
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            yc5047.cif
_cod_data_source_block           2oAPb_100K
_cod_database_code               1571597
_chemical_oxdiff_formula         'C20 H14 O2'
_olex2_refinement_description
;
;
_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 1.258
_oxdiff_exptl_absorpt_empirical_full_min 0.823