Triptycene-like naphthopleiadene as a readily accessible scaffold for supramolecular and materials chemistry.
Amin, Md Khairul; Ye, Chunchun; Pang, Shuhua; Liu, Yuancheng; Taylor, Dominic; Nichol, Gary S.; McKeown, Neil B.; Chemical science 15 (2024) 14968–14976; doi:10.1039/d4sc02755h

data_1572403
_publ_section_title
;
 Triptycene-like naphthopleiadene as a readily accessible scaffold for
 supramolecular and materials chemistry.
;
_journal_issue                   36
_journal_name_full               'Chemical science'
_journal_page_first              14968
_journal_page_last               14976
_journal_paper_doi               10.1039/d4sc02755h
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C32 H20 O4, 1.5[CH4O]'
_chemical_formula_sum            'C33.5 H26 O5.5'
_chemical_formula_weight         516.54
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-05
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-08-04 deposited with the CCDC.	2024-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                97.683(4)
_cell_angle_beta                 106.716(4)
_cell_angle_gamma                100.894(4)
_cell_formula_units_Z            2
_cell_length_a                   10.4986(5)
_cell_length_b                   11.6083(6)
_cell_length_c                   12.2425(6)
_cell_measurement_reflns_used    9071
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      29.1750
_cell_measurement_theta_min      3.8280
_cell_volume                     1374.87(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.892
_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    -87.00  12.00   1.00   30.00    --  -15.66 -22.00 -80.00   99
  2  \w    -43.00  56.00   1.00   30.00    --  -15.66  22.00  85.00   99
  3  \w    -54.00  45.00   1.00   30.00    --   17.38 -22.00 -80.00   99
  4  \w    -10.00  89.00   1.00   30.00    --   17.38  22.00  85.00   99
  5  \w    -39.00  11.00   1.00   30.00    --  -15.66 -77.00 120.00   50
  6  \w    -35.00  53.00   1.00   30.00    --  -15.66  38.00 150.00   88
  7  \w     -9.00  39.00   1.00   30.00    --   17.38  77.00  60.00   48
  8  \w     -9.00  39.00   1.00   30.00    --   17.38  77.00 -60.00   48
  9  \w     -9.00  39.00   1.00   30.00    --   17.38  77.00 -30.00   48
 10  \w     -9.00  39.00   1.00   30.00    --   17.38  77.00-120.00   48
 11  \w    -42.00  39.00   1.00   30.00    --  -15.66  77.00 -90.00   81
 12  \w    -20.00  56.00   1.00   30.00    --   17.38 -99.00  60.00   76
 13  \w    -20.00  56.00   1.00   30.00    --   17.38 -99.00-180.00   76
 14  \w     -9.00  39.00   1.00   30.00    --   17.38  77.00 150.00   48
 15  \w    -20.00  56.00   1.00   30.00    --   17.38 -99.00 -30.00   76
 16  \w    -20.00  56.00   1.00   30.00    --   17.38 -99.00 -90.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction XCalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0142266000
_diffrn_orient_matrix_UB_12      0.0630581000
_diffrn_orient_matrix_UB_13      0.0178976000
_diffrn_orient_matrix_UB_21      0.0686015000
_diffrn_orient_matrix_UB_22      0.0046945000
_diffrn_orient_matrix_UB_23      0.0007288000
_diffrn_orient_matrix_UB_31      -0.0192555000
_diffrn_orient_matrix_UB_32      0.0058906000
_diffrn_orient_matrix_UB_33      -0.0590850000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36195
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.328
_diffrn_reflns_theta_min         3.648
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           40.0
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99311
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       prism
_exptl_crystal_F_000             542
_exptl_crystal_recrystallization_method
'The material was recrystallised from methanol by slow cooling'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         6729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0626P)^2^+0.8917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5291
_reflns_number_total             6729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02755h2.cif
_cod_data_source_block           nm22008
_cod_depositor_comments
'Adding full bibliography for 1572402--1572407.cif.'
_cod_original_cell_volume        1374.87(12)
_cod_original_formula_sum        'C33.50 H26 O5.50'
_cod_database_code               1572403
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C32H20O4
_chemical_oxdiff_usercomment     '@ 120 K K71B49c'
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.985
_olex2_refinement_description
;
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 51 electrons were 
found in a volume of 404\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.5[CH4O] per Formula Unit 
which account for 54 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              69663
_shelx_hkl_checksum              91328
_shelx_fab_checksum              35818
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id K71B49c
_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 1.038
_oxdiff_exptl_absorpt_empirical_full_min 0.915