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_1572406
_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         'C30 H22 O4'
_chemical_formula_sum            'C30 H22 O4'
_chemical_formula_weight         446.507
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_atom_sites_solution_primary     direct
_audit_creation_date             2022-06-02
_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                90
_cell_angle_beta                 105.751(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9101(6)
_cell_length_b                   8.2287(3)
_cell_length_c                   14.3468(5)
_cell_measurement_reflns_used    7886
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      32.4080
_cell_measurement_theta_min      3.7910
_cell_volume                     2034.99(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  'olex2.refine 1.5-beta (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9973
_diffrn_measured_fraction_theta_max 0.9659
_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    -52.00  49.00   1.00   30.00    --   19.09 -70.00  34.00  101
  2  \w    -11.00  91.00   1.00   30.00    --   19.09  70.00 165.00  102
  3  \w    -42.00  14.00   1.00   30.00    --  -17.68 -77.00 -90.00   56
  4  \w    -40.00  55.00   1.00   30.00    --  -17.68  38.00 -60.00   95
  5  \w     -8.00  89.00   1.00   30.00    --   19.09  57.00 -60.00   97
  6  \w   -103.00 -58.00   1.00   30.00    --  -17.68 178.00-150.00   45
  7  \w     -3.00  92.00   1.00   30.00    --   19.09  38.00  60.00   95
  8  \w    -15.00  59.00   1.00   30.00    --   19.09 -99.00 120.00   74
  9  \w    -15.00  37.00   1.00   30.00    --   19.09 -99.00 -90.00   52
 10  \w    -15.00  59.00   1.00   30.00    --   19.09 -99.00-180.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0058823000
_diffrn_orient_matrix_UB_12      0.0743223000
_diffrn_orient_matrix_UB_13      0.0220279000
_diffrn_orient_matrix_UB_21      0.0320107000
_diffrn_orient_matrix_UB_22      0.0346012000
_diffrn_orient_matrix_UB_23      -0.0130823000
_diffrn_orient_matrix_UB_31      -0.0251819000
_diffrn_orient_matrix_UB_32      0.0265845000
_diffrn_orient_matrix_UB_33      -0.0445210000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.9973
_diffrn_reflns_Laue_measured_fraction_max 0.9659
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25275
_diffrn_reflns_point_group_measured_fraction_full 0.9973
_diffrn_reflns_point_group_measured_fraction_max 0.9659
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         32.57
_diffrn_reflns_theta_min         3.24
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91704
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       prism
_exptl_crystal_F_000             936.599
_exptl_crystal_recrystallization_method
'The material was recrystallised from dichloromethane by slow cooling'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.2517
_refine_diff_density_min         -0.2710
_refine_diff_density_rms         0.0673
_refine_ls_d_res_high            0.6601
_refine_ls_d_res_low             6.2848
_refine_ls_goodness_of_fit_ref   1.0922
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3569
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0922
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0070P)^2^+0.3672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0441
_refine_ls_wR_factor_ref         0.0465
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              25
_reflns_limit_h_min              -27
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                3083
_reflns_number_total             3569
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4sc02755h2.cif
_cod_data_source_block           NM22011
_cod_depositor_comments
'Adding full bibliography for 1572402--1572407.cif.'
_cod_original_cell_volume        2034.98(12)
_cod_database_code               1572406
_chemical_oxdiff_formula         C30H22O4
_chemical_oxdiff_usercomment     '@ 100 K K73B53c'
_olex2_refinement_description
;
;
_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 K73B53c
_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 1.221
_oxdiff_exptl_absorpt_empirical_full_min 0.833