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_1572407
_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         'C28 H18 O4, C3 H8 O'
_chemical_formula_sum            'C31 H26 O5'
_chemical_formula_weight         478.549
_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_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-11-15
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2021.11.04 svn.r5db059d7 for OlexSys, GUI svn.r6419)
;
_audit_update_record
;
2023-08-04 deposited with the CCDC.	2024-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                107.559(3)
_cell_angle_beta                 103.934(3)
_cell_angle_gamma                103.550(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2376(7)
_cell_length_b                   10.4837(6)
_cell_length_c                   12.0766(7)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      36.10
_cell_measurement_theta_min      2.26
_cell_volume                     1131.50(13)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       APEX4
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.9993
_diffrn_measured_fraction_theta_max 0.9936
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.9993
_diffrn_reflns_Laue_measured_fraction_max 0.9936
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            94416
_diffrn_reflns_point_group_measured_fraction_full 0.9993
_diffrn_reflns_point_group_measured_fraction_max 0.9936
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         36.38
_diffrn_reflns_theta_min         2.16
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.7202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1030 before and 0.0527 after correction.
The Ratio of minimum to maximum transmission is 0.9640.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       plate
_exptl_crystal_F_000             504.271
_exptl_crystal_recrystallization_method
'The material was recrystallised from isopropanol by slow evaporation'
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.153
_refine_diff_density_max         0.6082
_refine_diff_density_min         -0.3189
_refine_diff_density_rms         0.0798
_refine_ls_d_res_high            0.5992
_refine_ls_d_res_low             9.4293
_refine_ls_goodness_of_fit_ref   1.0588
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     559
_refine_ls_number_reflns         10949
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.0587
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          -0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+0.0726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0738
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -17
_reflns_limit_k_max              16
_reflns_limit_k_min              -17
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                8328
_reflns_number_total             10949
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4sc02755h2.cif
_cod_data_source_block           nm21004
_cod_depositor_comments
'Adding full bibliography for 1572402--1572407.cif.'
_cod_database_code               1572407
_olex2_refinement_description
;
1. Rigid body (RIGU) restrains
 H30, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 800'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id K48A197
_olex2_submission_special_instructions 'No special instructions were received'