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_7233408
_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           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 91.529(9)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   12.5556(11)
_cell_length_b                   10.9547(12)
_cell_length_c                   26.244(3)
_cell_measurement_reflns_used    2565
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      69.8580
_cell_measurement_theta_min      4.8480
_cell_volume                     3608.4(7)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2195
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0845286000
_diffrn_orient_matrix_UB_12      0.1020075000
_diffrn_orient_matrix_UB_13      -0.0012873000
_diffrn_orient_matrix_UB_21      0.0398780000
_diffrn_orient_matrix_UB_22      0.0440564000
_diffrn_orient_matrix_UB_23      0.0528671000
_diffrn_orient_matrix_UB_31      0.0796025000
_diffrn_orient_matrix_UB_32      0.0862429000
_diffrn_orient_matrix_UB_33      -0.0254762000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_av_unetI/netI     0.1428
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            21362
_diffrn_reflns_point_group_measured_fraction_full 0.855
_diffrn_reflns_point_group_measured_fraction_max 0.829
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.835
_diffrn_reflns_theta_min         3.369
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.955
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01) 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    1.349
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform'
_exptl_crystal_size_max          0.1898
_exptl_crystal_size_mid          0.1037
_exptl_crystal_size_min          0.022
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 1100 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -2.0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1033
_refine_ls_number_reflns         11741
_refine_ls_number_restraints     349
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.2173
_refine_ls_R_factor_gt           0.1143
_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^)+(0.1845P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2825
_refine_ls_wR_factor_ref         0.3860
_reflns_Friedel_coverage         0.604
_reflns_Friedel_fraction_full    0.698
_reflns_Friedel_fraction_max     0.661
_reflns_number_gt                4666
_reflns_number_total             11741
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01203f2.cif
_cod_data_source_block           500f1_chcl3
_cod_depositor_comments
'Adding full bibliography for 7233408--7233410.cif.'
_cod_original_cell_volume        3608.4(6)
_cod_database_code               7233408
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C11 H10 N O'
_chemical_oxdiff_usercomment     '100 K'
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.888
_reflns_odcompleteness_completeness 99.46
_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. Uiso/Uaniso restraints and constraints
Uanis(C16E) \\sim Ueq, Uanis(C9D) \\sim Ueq, Uanis(O1F) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 C15E, O1E, C17E, C1E, C18E, C2E, C14E, C3E, C13E, C4E, C12E, C16E, C5E, C11E,
 C9E, C6E, C10E, C8E, C7E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15F, O1F, C17F, C1F, C18F, C2F, C14F, C3F, C13F, C4F, C12F, C16F, C5F, C11F,
 C9F, C6F, C10F, C8F, C7F
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C4A(H4A), C6A(H6A), C7A(H7A), C8A(H8A), C10A(H10A), C11A(H11A),
 C13A(H13A), C14A(H14A), C3B(H3B), C4B(H4B), C6B(H6B), C7B(H7B), C8B(H8B),
 C10B(H10B), C11B(H11B), C13B(H13B), C14B(H14B), C3C(H3C), C4C(H4C), C6C(H6C),
 C7C(H7C), C8C(H8C), C10C(H10C), C11C(H11C), C13C(H13C), C14C(H14C), C3D(H3D),
 C4D(H4D), C6D(H6D), C7D(H7D), C8D(H8D), C10D(H10D), C11D(H11D), C13D(H13D),
 C14D(H14D), C3E(H3E), C4E(H4E), C6E(H6E), C7E(H7E), C8E(H8E), C10E(H10E),
 C11E(H11E), C13E(H13E), C14E(H14E), C3F(H3F), C4F(H4F), C6F(H6F), C7F(H7F),
 C8F(H8F), C10F(H10F), C11F(H11F), C13F(H13F), C14F(H14F)
4.b Idealised Me refined as rotating group:
 C18A(H18A,H18B,H18C), C18B(H18D,H18E,H18F), C18C(H18G,H18H,H18I), C18D(H18J,
 H18K,H18L), C18E(H18M,H18N,H18O), C18F(H18P,H18Q,H18R)
;
_shelx_res_checksum              25797
_olex2_date_sample_data_collection 2018-07-12
_olex2_submission_special_instructions 'No special instructions were received'