Helically twisted nanoribbons <i>via</i> stereospecific annulative π-extension reaction employing [7]helicene as a molecular wrench.
Swain, Asim; Radacki, Krzysztof; Braunschweig, Holger; Ravat, Prince; Chemical science 15 (2024) 11737–11747; doi:10.1039/d4sc01814a

data_1571754
_publ_section_title
;
 Helically twisted nanoribbons <i>via</i> stereospecific annulative
 &#x3c0;-extension reaction employing [7]helicene as a molecular wrench.
;
_journal_issue                   30
_journal_name_full               'Chemical science'
_journal_page_first              11737
_journal_page_last               11747
_journal_paper_doi               10.1039/d4sc01814a
_journal_volume                  15
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C80 H54, 3(C H2 Cl2)'
_chemical_formula_sum            'C83 H60 Cl6'
_chemical_formula_weight         1270.01
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           'CIF-fill 1.2z (K.Radacki, 2005-22)'
_audit_update_record
;
2023-12-18 deposited with the CCDC.	2024-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                114.189(3)
_cell_angle_beta                 109.595(3)
_cell_angle_gamma                93.418(2)
_cell_formula_units_Z            2
_cell_length_a                   14.6922(4)
_cell_length_b                   15.4658(4)
_cell_length_c                   16.5251(4)
_cell_measurement_reflns_used    10672
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.1630
_cell_measurement_theta_min      3.1690
_cell_volume                     3140.92(19)
_computing_cell_refinement       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 HPA
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HyPix Arc150'
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.900
_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    -81.00 -49.00   0.50    2.00    --  -65.03 -15.00-120.00   64
   2  \w     28.00  98.00   0.50    2.00    --   65.06   0.00  60.00  140
   3  \w     40.00 109.00   0.50    2.00    --   65.06  15.00 120.00  138
   4  \w     28.00  74.00   0.50    2.00    --   65.06 -95.00 120.00   92
   5  \w     36.00 109.00   0.50    2.00    --   65.06  15.00 -30.00  146
   6  \w     29.00  61.00   0.50    2.00    --   65.06 -95.00 150.00   64
   7  \w     30.00  69.00   0.50    2.00    --   65.06 -95.00   0.00   78
   8  \w     31.00  57.00   0.50    2.00    --   65.06 -95.00 -90.00   52
   9  \w     61.00  92.00   0.50    2.00    --   65.06-126.00 -90.00   62
  10  \w     28.00  61.00   0.50    2.00    --   65.06 -95.00-150.00   66
  11  \w     39.00  92.00   0.50    2.00    --   65.06-126.00  90.00  106
  12  \w     24.00  51.00   0.50    2.00    --   65.06-126.00 -90.00   54
  13  \w     59.00 108.00   0.50    2.00    --   65.06  15.00-120.00   98
  14  \w     36.00  70.00   0.50    2.00    --   71.48 -95.00  60.00   68
  15  \w   -102.00 -59.00   0.50    2.00    --  -73.64 126.00-150.00   86
  16  \w    -81.00 -48.00   0.50    2.00    --  -73.64 -15.00 -60.00   66
  17  \w   -110.00 -83.00   0.50    2.00    --  -73.64 -15.00 -60.00   54
  18  \w    -59.00 -30.00   0.50    2.00    --  -73.64 126.00  60.00   58
  19  \w   -102.00 -66.00   0.50    2.00    --  -73.64 126.00  60.00   72
  20  \w   -101.00 -35.00   0.50    2.00    --  -73.64 126.00-120.00  132
  21  \w   -101.00 -34.00   0.50    2.00    --  -75.71 126.00-180.00  134
  22  \w   -118.00 -74.00   0.50    2.00    --  -75.71-126.00 120.00   88
  23  \w    -89.00 -33.00   0.50    2.00    --  -75.71 126.00 -30.00  112
  24  \w   -117.00 -77.00   0.50    2.00    --  -75.71-126.00 -90.00   80
  25  \w   -120.00 -46.00   0.50    2.00    --  -75.71 -15.00  60.00  148
  26  \w   -115.00-112.50   0.50    2.00    --  -75.71-126.00  60.00    5

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31564
_diffrn_reflns_point_group_measured_fraction_full 0.681
_diffrn_reflns_point_group_measured_fraction_max 0.636
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.493
_diffrn_reflns_theta_min         3.191
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R X-ray Source'
_exptl_absorpt_coefficient_mu    2.862
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.57a (Rigaku Oxford Diffraction, 2022) Empirical 
absorption correction using spherical harmonics, implemented in SCALE3 
ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.003(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1648
_refine_ls_number_reflns         31564
_refine_ls_number_restraints     235
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0936
_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          0.2424
_refine_ls_wR_factor_ref         0.2691
_reflns_Friedel_coverage         0.414
_reflns_Friedel_fraction_full    0.408
_reflns_Friedel_fraction_max     0.372
_reflns_number_gt                24246
_reflns_number_total             31564
_reflns_threshold_expression     'I > 2\s(I)'
_twin_dimensionality             triperiodic
_twin_formation_mechanism        gt
_twin_morphology                 polysynthetic
_twin_special_details
;
 Component 2 rotated by 179.8918\% around [-0.01 0.90 -0.44] (reciprocal) or 
 [0.04 1.00 -0.04] (direct)
;
_cod_data_source_file            d4sc01814a3.cif
_cod_data_source_block           KR1104
_cod_depositor_comments
'Adding full bibliography for 1571753--1571754.cif.'
_cod_original_cell_volume        3140.90(17)
_cod_database_code               1571754
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.625
_shelx_estimated_absorpt_t_max   0.934
_shelx_res_checksum              28562