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_1571601
_publ_section_title
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 Evolution of structure and spectroscopic properties of a new
 1,3-diacetylpyrene polymorph with temperature and pressure.
;
_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
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 101.697(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.9685(2)
_cell_length_b                   10.7405(4)
_cell_length_c                   17.5252(6)
_cell_measurement_reflns_used    5171
_cell_measurement_temperature    298
_cell_measurement_theta_max      18.4030
_cell_measurement_theta_min      1.7740
_cell_volume                     1284.44(8)
_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)'
_diffrn_ambient_temperature      298.15
_diffrn_crystal_treatment
'pressurized rapidly in silicone oil as a hydrostatic medium'
_diffrn_measured_fraction_theta_full 0.8194
_diffrn_measured_fraction_theta_max 0.7668
_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    -43.00  41.00   1.00    1.00    --    0.00   0.00   0.00   84
  2  \w    -43.00  41.00   1.00    5.00    --    0.00   0.00   0.00   84
  3  \w    -43.00  41.00   1.00    1.00    --    0.00  30.00   0.00   84
  4  \w    -43.00  41.00   1.00    5.00    --    0.00  30.00   0.00   84
  5  \w    -43.00  41.00   1.00    1.00    --    0.00  90.00   0.00   84
  6  \w    -43.00  41.00   1.00    5.00    --    0.00  90.00   0.00   84
;
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41618
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.8194
_diffrn_reflns_Laue_measured_fraction_max 0.7668
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33624
_diffrn_reflns_point_group_measured_fraction_full 0.8194
_diffrn_reflns_point_group_measured_fraction_max 0.7668
_diffrn_reflns_theta_full        14.4602
_diffrn_reflns_theta_max         18.68
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.041
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.998
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43d (Rigaku Oxford Diffraction, 2018)
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            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       irregular
_exptl_crystal_F_000             600.009
_exptl_crystal_preparation
'Mounted in a Diamond-Anvil Cell using silicone oil as pressure medium.'
_exptl_crystal_pressure_history  'Pressurized to 0.85 GPa.'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.1950
_refine_diff_density_min         -0.2133
_refine_diff_density_rms         0.0519
_refine_ls_d_res_high            0.6497
_refine_ls_d_res_low             6.8238
_refine_ls_goodness_of_fit_ref   1.0541
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     375
_refine_ls_number_reflns         3765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0541
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+0.0330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0809
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                2613
_reflns_number_total             3765
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            yc5047.cif
_cod_data_source_block           2oAPb_0p85GPa_HAR_anh
_cod_database_code               1571601
_olex2_refine_details
;
Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by 
employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       ORCA 5.0
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         B3LYP
   BASIS SET:      6-311G(d,p)
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2024-02-20_12-26-43
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