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_2108399
_publ_section_title
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 Structure and piezochromism of pyrene-1-carbaldehyde at high pressure
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_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
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_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             2018-06-25
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                109.37(3)
_cell_angle_beta                 99.57(3)
_cell_angle_gamma                100.71(3)
_cell_formula_units_Z            2
_cell_length_a                   6.477(2)
_cell_length_b                   8.041(2)
_cell_length_c                   10.205(3)
_cell_measurement_reflns_used    460
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.6140
_cell_measurement_theta_min      1.9140
_cell_volume                     477.6(3)
_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)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.718
_diffrn_measured_fraction_theta_max 0.520
_diffrn_measurement_details
'#__ type_ start__ end____ width___ exp.time_ 1 omega -150.00 -94.00 0.2000 0.3970 omega____ theta____ kappa____ phi______ frames - -20.0000 70.0000 -24.2319 280 #__ type_ start__ end____ width___ exp.time_ 2 omega -150.00 -94.00 0.2000 0.3970 omega____ theta____ kappa____ phi______ frames - -20.0000 70.0000 155.7681 280 #__ type_ start__ end____ width___ exp.time_ 3 omega -105.00 -76.00 0.2000 0.3970 omega____ theta____ kappa____ phi______ frames - 20.0000 70.0000 155.7700 145 #__ type_ start__ end____ width___ exp.time_ 4 omega -105.00 -75.00 0.2000 0.3970 omega____ theta____ kappa____ phi______ frames - 20.0000 70.0000 -24.2300 150 #__ type_ start__ end____ width___ exp.time_ 5 omega -96.00 -30.00 0.2000 0.3970 omega____ theta____ kappa____ phi______ frames - 20.0000 -70.0000 24.2300 330 #__ type_ start__ end____ width___ exp.time_ 6 omega -103.00 -66.00 0.2000 0.3970 omega____ theta____ kappa____ phi______ frames - -20.0000 -70.0000 -155.7700 185 #__ type_ start__ end____ width___ exp.time_ 7 omega -103.80 -66.00 0.2000 0.3970 omega____ theta____ kappa____ phi______ frames - -20.0000 -70.0000 24.2300 189 #__ type_ start__ end____ width___ exp.time_ 8 omega -96.00 -30.00 0.2000 0.3970 omega____ theta____ kappa____ phi______ frames - 20.0000 -70.0000 -155.7700 330'
_diffrn_measurement_device       'abstract diffractometer'
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'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0506264000
_diffrn_orient_matrix_UB_12      0.0235626000
_diffrn_orient_matrix_UB_13      -0.0250498000
_diffrn_orient_matrix_UB_21      0.0590807000
_diffrn_orient_matrix_UB_22      0.0320340000
_diffrn_orient_matrix_UB_23      -0.0134875000
_diffrn_orient_matrix_UB_31      -0.0123243000
_diffrn_orient_matrix_UB_32      -0.0530677000
_diffrn_orient_matrix_UB_33      -0.0436105000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4859
_diffrn_reflns_av_R_equivalents  0.1391
_diffrn_reflns_av_unetI/netI     0.0786
_diffrn_reflns_Laue_measured_fraction_full 0.718
_diffrn_reflns_Laue_measured_fraction_max 0.520
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2461
_diffrn_reflns_point_group_measured_fraction_full 0.718
_diffrn_reflns_point_group_measured_fraction_max 0.520
_diffrn_reflns_theta_full        16.950
_diffrn_reflns_theta_max         22.567
_diffrn_reflns_theta_min         1.900
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.051
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.07393
_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_density_diffrn    1.601
_exptl_crystal_description
;
;
_exptl_crystal_F_000             240
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2461
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.2634
_refine_ls_R_factor_gt           0.1689
_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^)+(0.1308P)^2^+1.3113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3776
_refine_ls_wR_factor_ref         0.4342
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1176
_reflns_number_total             2461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            xk5054sup1.cif
_cod_data_source_block           28kbar
_cod_original_cell_volume        477.5(3)
_cod_database_code               2108399
_cod_database_fobs_code          2108399
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C17 H10 O1'
_diffrn_oxdiff_twin_integration_method simultaneous
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.725(6)
 0.237(6) 0.0377(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C14(H14), C8(H8), C6(H6), C7(H7), C4(H4), C13(H13), C11(H11),
 C17(H17), C10(H10)
;
_shelx_res_checksum              60897
_shelx_hkl_checksum              94108
_olex2_submission_special_instructions 'No special instructions were received'