Triptycene-grafted helicenes: modular synthesis and key properties
Vacek, Martin; Kutsenka, Katsiaryna; Stará, Irena G; Stary, I.; Seankongsuk, Pattarakiat; Rybáček, Jiří; Vacek, Jaroslav; Bednárová, Lucie; Pohl, Radek; Cisarova, Ivana; Chemical Communications  (2026) –; doi:10.1039/D5CC06240C

data_7135714
_publ_section_title
;
 Triptycene-grafted helicenes: modular synthesis and key properties.
;
_journal_issue                   33
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8426
_journal_page_last               8430
_journal_paper_doi               10.1039/d5cc06240c
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         'C66 H38, 3(C4 H8 O)'
_chemical_formula_sum            'C78 H62 O3'
_chemical_formula_weight         1047.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;FinalCif 2024.9-1 by Daniel Kratzert, Freiburg 2025, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2025-10-01 deposited with the CCDC.	2026-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.047(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0567(6)
_cell_length_b                   15.9953(7)
_cell_length_c                   44.136(2)
_cell_measurement_reflns_used    9651
_cell_measurement_temperature    100.14999999999998
_cell_measurement_theta_max      72.1855
_cell_measurement_theta_min      2.9384
_cell_measurement_wavelength     1.54178
_cell_volume                     5679.7(6)
_computing_cell_refinement       'SAINT V8.41 (Bruker AXS LLC)'
_computing_data_collection       'Bruker Instrument Service v8.5.5.6'
_computing_data_reduction        'SAINT V8.41 (Bruker AXS LLC)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1503)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'XS, VERSION 2013/1'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.391
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;<Phi   scan: start= 360.0; len= 180.0; end= 540.0 at [Counterclockwise Eulerian 
angles: dx= 60.00 mm theta=  25.000 deg omega= 360.000 deg chi=  54.740 deg] 
measure for 3.0 seconds; frame angle 1.00 degrees, wavelength=1.54184>
<Phi   scan: start= 360.0; len= 180.0; end= 540.0 at [Counterclockwise Eulerian 
angles: dx= 45.00 mm theta=  27.500 deg omega= 360.000 deg chi=  54.740 deg] 
measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=1.54184>
<Phi   scan: start= 180.0; len= 180.0; end= 360.0 at [Counterclockwise Eulerian 
angles: dx= 45.00 mm theta=  27.500 deg omega= 360.000 deg chi=  54.740 deg] 
measure for 1.0 seconds; frame angle 1.00 degrees, wavelength=1.54184>
<Phi   scan: start= 166.7; len= 322.5; end= 489.2 at [Counterclockwise Eulerian 
angles: dx= 70.00 mm theta=  60.846 deg omega=  20.551 deg chi=  24.000 deg] 
measure for 15.0 seconds; frame angle 0.30 degrees, wavelength=1.54184>
<Phi   scan: start= 360.0; len=   0.3; end= 360.3 at [Counterclockwise Eulerian 
angles: dx= 70.00 mm theta=  38.346 deg omega=  55.438 deg chi= -44.500 deg] 
measure for 9.0 seconds; frame angle 0.30 degrees, wavelength=1.54184>
<Omega scan: start=   4.5; len=  75.0; end=  79.5 at [Counterclockwise Eulerian 
angles: dx= 70.00 mm theta=  60.846 deg phi= 180.000 deg chi=  68.500 deg] 
measure for 15.0 seconds; frame angle 0.30 degrees, wavelength=1.54184>
<Omega scan: start=   1.1; len= 105.3; end= 106.4 at [Counterclockwise Eulerian 
angles: dx= 70.00 mm theta=  60.846 deg phi=  27.000 deg chi=  65.500 deg] 
measure for 15.0 seconds; frame angle 0.30 degrees, wavelength=1.54184>
<Phi   scan: start= 204.0; len= 192.0; end= 396.0 at [Counterclockwise Eulerian 
angles: dx= 70.00 mm theta= -16.952 deg omega= 347.411 deg chi=  44.500 deg] 
measure for 6.0 seconds; frame angle 0.30 degrees, wavelength=1.54184>
<Omega scan: start=   1.1; len= 105.3; end= 106.4 at [Counterclockwise Eulerian 
angles: dx= 70.00 mm theta=  60.846 deg phi= 324.000 deg chi=  65.500 deg] 
measure for 15.0 seconds; frame angle 0.30 degrees, wavelength=1.54184>
<Omega scan: start=   1.1; len= 105.3; end= 106.4 at [Counterclockwise Eulerian 
angles: dx= 70.00 mm theta=  60.846 deg phi= 162.000 deg chi=  65.500 deg] 
measure for 15.0 seconds; frame angle 0.30 degrees, wavelength=1.54184>
<Omega scan: start=   1.1; len= 105.3; end= 106.4 at [Counterclockwise Eulerian 
angles: dx= 70.00 mm theta=  60.846 deg phi= 270.000 deg chi=  65.500 deg] 
measure for 15.0 seconds; frame angle 0.30 degrees, wavelength=1.54184>
<Phi   scan: start= 204.0; len= 183.9; end= 387.9 at [Counterclockwise Eulerian 
angles: dx= 70.00 mm theta=  43.392 deg omega= 345.643 deg chi=  24.000 deg] 
measure for 10.0 seconds; frame angle 0.30 degrees, wavelength=1.54184>
<Omega scan: start=   1.1; len= 105.3; end= 106.4 at [Counterclockwise Eulerian 
angles: dx= 70.00 mm theta=  60.846 deg phi=  81.000 deg chi=  65.500 deg] 
measure for 15.0 seconds; frame angle 0.30 degrees, wavelength=1.54184>
<Omega scan: start=   1.1; len= 105.3; end= 106.4 at [Counterclockwise Eulerian 
angles: dx= 70.00 mm theta=  60.846 deg phi= 243.000 deg chi=  65.500 deg] 
measure for 15.0 seconds; frame angle 0.30 degrees, wavelength=1.54184>
<Omega scan: start=   1.1; len= 105.3; end= 106.4 at [Counterclockwise Eulerian 
angles: dx= 70.00 mm theta=  60.846 deg phi=  54.000 deg chi=  65.500 deg] 
measure for 15.0 seconds; frame angle 0.30 degrees, wavelength=1.54184>
<Omega scan: start=   1.1; len= 105.3; end= 106.4 at [Counterclockwise Eulerian 
angles: dx= 70.00 mm theta=  60.846 deg phi= 216.000 deg chi=  65.500 deg] 
measure for 15.0 seconds; frame angle 0.30 degrees, wavelength=1.54184>
<Omega scan: start=   1.1; len= 105.3; end= 106.4 at [Counterclockwise Eulerian 
angles: dx= 70.00 mm theta=  60.846 deg phi= 360.000 deg chi=  65.500 deg] 
measure for 15.0 seconds; frame angle 0.30 degrees, wavelength=1.54184>
<Omega scan: start=   1.1; len= 105.3; end= 106.4 at [Counterclockwise Eulerian 
angles: dx= 70.00 mm theta=  60.846 deg phi= 297.000 deg chi=  65.500 deg] 
measure for 15.0 seconds; frame angle 0.30 degrees, wavelength=1.54184>
<Omega scan: start=   4.5; len=  75.0; end=  79.5 at [Counterclockwise Eulerian 
angles: dx= 70.00 mm theta=  60.846 deg phi= 108.000 deg chi=  68.500 deg] 
measure for 15.0 seconds; frame angle 0.30 degrees, wavelength=1.54184>
;
_diffrn_measurement_device       'KAPPA diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            54188
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_reduction_process narrow-frame
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.271
_diffrn_reflns_theta_min         2.005
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.1
_diffrn_source_target            Cu
_diffrn_source_type              'INCOATEC I\mS Diamond II'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for single-crystal
 structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            colourless_yellow
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       plate
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.329
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         54188
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.1368
_refine_ls_R_factor_gt           0.1342
_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^)+(0.0305P)^2^+23.0588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3248
_refine_ls_wR_factor_ref         0.3258
_reflns_Friedel_coverage         0.000
_reflns_number_gt                51957
_reflns_number_total             54188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06240c10.cif
_cod_data_source_block           cu_psy_k358e_stary_tw
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7135714.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7135714
_shelx_shelxl_version_number     2019/3
_exptl_bruker_absorpt_correction_t_ratio 0.809
_shelx_estimated_absorpt_t_min   0.837
_shelx_estimated_absorpt_t_max   0.951
_bruker_diffrn_measurement_temperature_device 'Oxford Cryostream 1000'
_diffrn_measurement_bruker_total_exposure_time 97945.0
_diffrn_reflns_bruker_av_norm_i  34946.265
_diffrn_reflns_bruker_number_gt  64262
_computing_bruker_data_scaling
'SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction'
_geom_details
; All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
_shelx_res_checksum              73848
_shelx_hkl_checksum              27525