Polymorphism and resulting luminescence properties of 1-acetylpyrene
Tchoń, Daniel; Trzybiński, Damian; Wrona-Piotrowicz, Anna; Makal, Anna; CrystEngComm 21 (2019) 5845–; doi:10.1039/C9CE01203F

data_7233409
_publ_section_title
;
 Polymorphism and resulting luminescence properties of 1-acetylpyrene
;
_journal_issue                   38
_journal_name_full               CrystEngComm
_journal_page_first              5845
_journal_paper_doi               10.1039/C9CE01203F
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C18 H12 O'
_chemical_formula_sum            'C18 H12 O'
_chemical_formula_weight         244.28
_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_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-05-03
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-23 deposited with the CCDC.    2019-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.218(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4667(6)
_cell_length_b                   11.5284(4)
_cell_length_c                   10.3816(5)
_cell_measurement_reflns_used    1999
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      69.1930
_cell_measurement_theta_min      4.3590
_cell_volume                     1214.32(11)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4391
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.951
_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 -44.00 102.00 1.00 1.00 -- 0.00 77.00 -90.00 146 2 \w -102.00 -35.00 1.00 1.00 -- 0.00-178.00-180.00 67 3 \w -152.00 -80.00 1.00 1.50 -- -55.06 -94.00 150.00 72 4 \w -152.00 -80.00 1.00 1.50 -- -55.06 -94.00 -60.00 72 5 \w -98.00 40.00 1.00 1.50 -- -55.06 61.00 150.00 138 6 \w -96.00 -2.00 1.00 1.50 -- -55.06 125.00 150.00 94 7 \w 23.00 122.00 1.00 1.50 -- 55.06-125.00-120.00 99 8 \w 11.00 147.00 1.00 1.50 -- 55.06 45.00 30.00 136 9 \w 94.00 147.00 1.00 1.50 -- 55.06 125.00 30.00 53 10 \w 100.00 178.00 1.00 4.50 -- 110.13 111.00 0.00 78 11 \w 67.00 178.00 1.00 4.50 -- 110.13 50.00 -30.00 111 12 \w 57.00 151.00 1.00 4.50 -- 110.13 178.00-150.00 94 13 \w 8.00 148.00 1.00 4.50 -- 110.13 -77.00 -30.00 140 14 \w 17.00 115.00 1.00 4.50 -- 110.13-111.00-150.00 98 15 \w 67.00 178.00 1.00 4.50 -- 110.13 63.00 30.00 111 16 \w 17.00 115.00 1.00 4.50 -- 110.13-111.00 -30.00 98 17 \w 17.00 78.00 1.00 4.50 -- 110.13-111.00 -60.00 61'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1494846000
_diffrn_orient_matrix_UB_12      0.0183367000
_diffrn_orient_matrix_UB_13      -0.0534491000
_diffrn_orient_matrix_UB_21      0.0262920000
_diffrn_orient_matrix_UB_22      0.0833793000
_diffrn_orient_matrix_UB_23      -0.1065738000
_diffrn_orient_matrix_UB_31      -0.0053500000
_diffrn_orient_matrix_UB_32      -0.1028271000
_diffrn_orient_matrix_UB_33      -0.0959126000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7828
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.041
_diffrn_reflns_theta_min         4.358
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.485
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       plate
_exptl_crystal_F_000             512
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methylene chloride / n-hexane'
_exptl_crystal_size_max          0.388
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.016
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2231
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0859P)^2^+0.1536P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1700
_reflns_number_total             2231
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01203f2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7233408--7233410.cif.'
_cod_database_code               7233409
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C18 H12 O'
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.791
_reflns_odcompleteness_completeness 98.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C)
;
_shelx_res_checksum              50340
_olex2_date_sample_data_collection 2017-11-11
_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 2.090
_oxdiff_exptl_absorpt_empirical_full_min 0.680