Statically and dynamically flexible hydrogen-bonded frameworks based on 4,5,9,10-tetrakis(4-carboxyphenyl)pyrene.
Hashimoto, Taito; Oketani, Ryusei; Inoue, Asato; Okubo, Kohei; Oka, Kouki; Tohnai, Norimitsu; Kamiya, Kazuhide; Nakanishi, Shuji; Hisaki, Ichiro; Chemical communications (Cambridge, England) 59 (2023) 7224–7227; doi:10.1039/d3cc01877f

data_7131673
_publ_section_title
;
 Statically and dynamically flexible hydrogen-bonded frameworks based on
 4,5,9,10-tetrakis(4-carboxyphenyl)pyrene.
;
_journal_issue                   47
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7224
_journal_page_last               7227
_journal_paper_doi               10.1039/d3cc01877f
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C44 H26 O8'
_chemical_formula_sum            'C44 H26 O8'
_chemical_formula_weight         682.65
_chemical_name_systematic        CP-Py-3
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-08-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-04-12 deposited with the CCDC.	2023-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                78.06(2)
_cell_angle_beta                 86.453(17)
_cell_angle_gamma                67.84(2)
_cell_formula_units_Z            1
_cell_length_a                   7.5864(17)
_cell_length_b                   9.404(3)
_cell_length_c                   13.016(3)
_cell_measurement_reflns_used    1639
_cell_measurement_temperature    113
_cell_measurement_theta_max      31.3690
_cell_measurement_theta_min      2.7340
_cell_volume                     841.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      113
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.846
_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    -90.00  90.00   1.00    5.00    --   25.00  45.00   0.00  180
  2  \w    -90.00  90.00   1.00    5.00    --   25.00  45.00  90.00  180
  3  \w    -90.00  90.00   1.00    5.00    --   25.00  45.00 180.00  180
  4  \w    -90.00  90.00   1.00    5.00    --   25.00  45.00 270.00  180
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0971248000
_diffrn_orient_matrix_UB_12      -0.0165114000
_diffrn_orient_matrix_UB_13      0.0138474000
_diffrn_orient_matrix_UB_21      -0.0553177000
_diffrn_orient_matrix_UB_22      0.0904250000
_diffrn_orient_matrix_UB_23      0.0057052000
_diffrn_orient_matrix_UB_31      -0.0289329000
_diffrn_orient_matrix_UB_32      0.0240504000
_diffrn_orient_matrix_UB_33      -0.0619122000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.81111
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.846
_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       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8327
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_theta_full        29.122
_diffrn_reflns_theta_max         33.101
_diffrn_reflns_theta_min         1.825
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       plate
_exptl_crystal_F_000             354
_exptl_crystal_recrystallization_method
'obtained by desolvation-triggered structural transformation'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.114
_refine_ls_R_factor_all          0.2777
_refine_ls_R_factor_gt           0.2112
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5583
_refine_ls_wR_factor_ref         0.5974
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1777
_reflns_number_total             3644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01877f2.cif
_cod_data_source_block           CP-Py-3
_cod_depositor_comments
'Adding full bibliography for 7131672--7131678.cif.'
_cod_original_cell_volume        841.2(4)
_cod_database_code               7131673
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.987
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00B(H00B), C00F(H00F), C00H(H00H), C00I(H00I), C00J(H00J),
 C00K(H00K), C00L(H00L), C00M(H00M), C00P(H00P), C00Q(H00Q)
2.b Idealised tetrahedral OH refined as rotating group:
 O001(H001), O003(H003)
;
_shelx_res_checksum              97269
_shelx_hkl_checksum              49163
_shelx_fab_checksum              95704
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_original_sample_id CPPy-Form3
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.474
_oxdiff_exptl_absorpt_empirical_full_min 0.525