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_1571599
_publ_section_title
;
 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                 103.701(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.2350(3)
_cell_length_b                   11.2573(4)
_cell_length_c                   17.7365(5)
_cell_measurement_reflns_used    3144
_cell_measurement_temperature    287(11)
_cell_measurement_theta_max      77.0770
_cell_measurement_theta_min      4.6850
_cell_volume                     1403.47(9)
_diffrn_ambient_temperature      293(1)
_diffrn_measured_fraction_theta_full 0.9905
_diffrn_measured_fraction_theta_max 0.9769
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.9905
_diffrn_reflns_Laue_measured_fraction_max 0.9769
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9192
_diffrn_reflns_point_group_measured_fraction_full 0.9905
_diffrn_reflns_point_group_measured_fraction_max 0.9769
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         77.61
_diffrn_reflns_theta_min         4.69
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.70a (Rigaku Oxford Diffraction, 2022)
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    1.355
_exptl_crystal_description       plate
_exptl_crystal_F_000             601.956
_refine_diff_density_max         0.2413
_refine_diff_density_min         -0.1948
_refine_diff_density_rms         0.0558
_refine_ls_d_res_high            0.7893
_refine_ls_d_res_low             9.4244
_refine_ls_goodness_of_fit_ref   0.8879
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     375
_refine_ls_number_reflns         2912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.8879
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.2842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -9
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                2233
_reflns_number_total             2912
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            yc5047.cif
_cod_data_source_block           2oAPb_293K_HAR_anh
_cod_database_code               1571599
_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:      6-31G(d,p)
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2024-02-20_12-37-39
;