Structure and piezochromism of pyrene-1-carbaldehyde at high pressure
Tchoń, Daniel; Makal, Anna; Acta Crystallographica Section B 75 (2019) –; doi:10.1107/S2052520619003354

data_2108394
_publ_section_title
;
 Structure and piezochromism of pyrene-1-carbaldehyde at high pressure
;
_journal_coeditor_code           XK5054SUP1
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520619003354
_journal_volume                  75
_journal_year                    2019
_chemical_formula_moiety         'C17 H10 O'
_chemical_formula_sum            'C17 H10 O'
_chemical_formula_weight         230.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-01-18
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                109.898(2)
_cell_angle_beta                 98.9790(19)
_cell_angle_gamma                100.773(2)
_cell_formula_units_Z            2
_cell_length_a                   6.92715(15)
_cell_length_b                   8.3336(2)
_cell_length_c                   10.4706(2)
_cell_measurement_reflns_used    16541
_cell_measurement_temperature    278.55(10)
_cell_measurement_theta_max      45.2170
_cell_measurement_theta_min      2.6730
_cell_volume                     542.32(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      278.55(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0026
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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    -69.00  21.00   1.00    4.00    --    0.00 -57.00-120.00   90
  2  \w    -26.00  72.00   1.00    4.00    --    0.00  37.00  30.00   98
  3  \w    -73.00  73.00   1.00    4.00    --    0.00   0.00-180.00  146
  4  \w    -26.00  72.00   1.00    4.00    --    0.00  37.00-180.00   98
  5  \w    -20.00  42.00   1.00    4.00    --    0.00 -99.00 -30.00   62
  6  \w    -20.00  42.00   1.00    4.00    --    0.00 -99.00 -90.00   62
  7  \w    -39.00  10.00   1.00    4.00    --   10.00 111.00  82.11   49
  8  \w    -17.00  18.00   1.00    4.00    --   26.00 101.00 -59.69   35
  9  \w     -1.00  27.00   1.00   16.00    --   38.00  93.00 112.47   28
 10  \w      6.00  33.00   1.00   16.00    --   42.00  88.00  35.36   27
 11  \w      7.00  35.00   1.00   16.00    --   42.00  86.00 -45.71   28
 12  \w     13.00  40.00   1.00   16.00    --   46.00  83.00-125.74   27
 13  \w     13.00  45.00   1.00   16.00    --   46.00  82.00 176.80   32
 14  \w     17.00  45.00   1.00   16.00    --   50.00  82.00  42.28   28
 15  \w     17.00  45.00   1.00   16.00    --   50.00  82.00 113.27   28
 16  \w     17.00  45.00   1.00   16.00    --   50.00  82.00 -81.05   28
 17  \w     17.00  45.00   1.00   16.00    --   50.00  82.00 -21.36   28
 18  \w     17.00  45.00   1.00   16.00    --   50.00  82.00  76.48   28
 19  \w     27.00 127.00   1.00   16.00    --   56.79  77.00-120.00  100
 20  \w     27.00 127.00   1.00   16.00    --   56.79  77.00 120.00  100
 21  \w     27.00 127.00   1.00   16.00    --   56.79  77.00 -90.00  100
 22  \w    -13.00  87.00   1.00   16.00    --   56.79 -77.00-180.00  100
 23  \w    -12.00  78.00   1.00   16.00    --   56.79 -57.00  90.00   90
 24  \w     27.00 127.00   1.00   16.00    --   56.79  77.00-150.00  100
 25  \w     73.00 128.00   1.00   16.00    --   56.79 125.00  60.00   55
 26  \w    -13.00  87.00   1.00   16.00    --   56.79 -77.00  90.00  100
 27  \w      2.00 114.00   1.00   16.00    --   56.79-125.00  30.00  112
 28  \w     27.00 127.00   1.00   16.00    --   56.79  77.00 -30.00  100
 29  \w    -12.00  78.00   1.00   16.00    --   56.79 -57.00   0.00   90
 30  \w    -13.00  87.00   1.00   16.00    --   56.79 -77.00-120.00  100
 31  \w     27.00 127.00   1.00   16.00    --   56.79  77.00 -60.00  100
 32  \w     27.00 127.00   1.00   16.00    --   56.79  77.00   0.00  100
 33  \w     27.00 127.00   1.00   16.00    --   56.79  77.00 150.00  100
 34  \w     27.00 127.00   1.00   16.00    --   56.79  77.00-180.00  100
 35  \w     27.00 127.00   1.00   16.00    --   56.79  77.00  60.00  100
 36  \w     27.00 111.00   1.00   16.00    --   56.79  77.00  30.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0346725000
_diffrn_orient_matrix_UB_12      0.0543025000
_diffrn_orient_matrix_UB_13      -0.0330074000
_diffrn_orient_matrix_UB_21      -0.1007593000
_diffrn_orient_matrix_UB_22      -0.0515681000
_diffrn_orient_matrix_UB_23      -0.0155587000
_diffrn_orient_matrix_UB_31      -0.0126852000
_diffrn_orient_matrix_UB_32      0.0563189000
_diffrn_orient_matrix_UB_33      0.0645740000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            54427
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         45.386
_diffrn_reflns_theta_min         2.130
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
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    1.410
_exptl_crystal_description       plate
_exptl_crystal_F_000             240
_exptl_crystal_size_max          0.356
_exptl_crystal_size_mid          0.288
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         9109
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0843P)^2^+0.0851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1654
_refine_ls_wR_factor_ref         0.1793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6621
_reflns_number_total             9109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            xk5054sup1.cif
_cod_data_source_block           0kbar
_cod_database_code               2108394
_cod_database_fobs_code          2108394
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C17 H10 O'
_chemical_oxdiff_usercomment     'thick yellow plate'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     45.18
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(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), C17(H17)
;
_shelx_res_checksum              30332
_shelx_hkl_checksum              55540
_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 1.419
_oxdiff_exptl_absorpt_empirical_full_min 0.613