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_1571753
_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_formula_moiety         'C68 H70, 2(C H2 Cl2)'
_chemical_formula_sum            'C70 H74 Cl4'
_chemical_formula_weight         1057.09
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-07-19
_audit_creation_method           'CIF-fill 1.3e (K.Radacki, 2005-22)'
_audit_update_record
;
2023-12-18 deposited with the CCDC.	2024-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                66.4050(10)
_cell_angle_beta                 76.5680(10)
_cell_angle_gamma                74.1110(10)
_cell_formula_units_Z            2
_cell_length_a                   14.16160(10)
_cell_length_b                   14.61250(10)
_cell_length_c                   15.92860(10)
_cell_measurement_reflns_used    74644
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.5530
_cell_measurement_theta_min      3.0540
_cell_volume                     2876.94(4)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 HPA
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HyPix Arc150'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
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  1  \w     29.00  54.00   0.50    0.50    --   58.61 -95.00 -77.00   50
  2  \w    -56.00 -30.00   0.50    0.50    --  -60.19  95.00  32.00   52
  3  \w    -76.00 -51.00   0.50    0.50    --  -69.72  95.00  32.00   50
  4  \w     30.00  56.00   0.50    0.50    --   71.30 -95.00 -77.00   52
  5  \w    -84.00 -58.00   0.50    1.10    --  -76.37  95.00  32.00   52
  6  \w     40.00  65.00   0.50    1.10    --   82.31 -95.00 -77.00   50
  7  \w     12.00  37.00   0.50    0.50    --    2.00  66.00  68.04   50
  8  \w     12.00  37.00   0.50    0.50    --    2.00  66.00 171.80   50
  9  \w     16.00  41.00   0.50    0.50    --    6.00  65.00 -96.15   50
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 11  \w     16.00  41.00   0.50    0.50    --    6.00  65.00-162.60   50
 12  \w     17.00  42.00   0.50    0.50    --    6.00  64.00 106.85   50
 13  \w     17.00  42.00   0.50    0.50    --    6.00  64.00 -19.08   50
 14  \w     21.00  46.00   0.50    0.50    --   10.00  62.00   7.10   50
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 17  \w     25.00  50.00   0.50    0.50    --   14.00  61.00 133.43   50
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 19  \w    -48.00 -23.00   0.50    0.50    --  -18.00 130.00  45.23   50
 20  \w     30.00  55.00   0.50    0.50    --   18.00  60.00  90.24   50
 21  \w     30.00  55.00   0.50    0.50    --   18.00  59.00 -82.54   50
 22  \w     30.00  55.00   0.50    0.50    --   18.00  60.00-164.10   50
 23  \w     30.00  55.00   0.50    0.50    --   18.00  58.00 163.50   50
 24  \w     34.00  59.00   0.50    0.50    --   22.00  58.00  -4.96   50
 25  \w     34.00  59.00   0.50    0.50    --   22.00  58.00 -55.35   50
 26  \w     34.00  59.00   0.50    0.50    --   22.00  58.00 139.61   50
 27  \w     34.00  59.00   0.50    0.50    --   22.00  59.00-101.14   50
 28  \w     34.00  59.00   0.50    0.50    --   22.00  57.00 -28.76   50
 29  \w     34.00  59.00   0.50    0.50    --   22.00  59.00 107.65   50
 30  \w     34.00  59.00   0.50    0.50    --   22.00  57.00  43.73   50
 31  \w     34.00  59.00   0.50    0.50    --   22.00  57.00  66.73   50
 32  \w     34.00  59.00   0.50    0.50    --   22.00  57.00-124.00   50
 33  \w     34.00  59.00   0.50    0.50    --   22.00  59.00  14.55   50
 34  \w    -64.00 -39.00   0.50    0.50    --  -26.00 -51.00-149.29   50
 35  \w     39.00  64.00   0.50    0.50    --   26.00  52.00-154.61   50
 36  \w     39.00  64.00   0.50    0.50    --   26.00  52.00-100.33   50
 37  \w    -74.00 -48.00   0.50    0.50    --  -30.00 -47.00 -98.58   52
 38  \w    -74.00 -48.00   0.50    0.50    --  -34.00 -52.00   4.70   52
 39  \w    -74.00 -48.00   0.50    0.50    --  -34.00 -51.00-102.28   52
 40  \w     47.00  72.00   0.50    0.50    --   34.00  52.00 175.65   50
 41  \w     48.00  73.00   0.50    0.50    --   34.00  51.00 -37.60   50
 42  \w     48.00  73.00   0.50    0.50    --   34.00  51.00 165.67   50
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 45  \w    -79.00 -53.00   0.50    0.50    --  -38.00 -50.00  34.10   52
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 52  \w     51.00  76.00   0.50    0.50    --   38.00  52.00 -84.42   50
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 54  \w     55.00  80.00   0.50    0.50    --   42.00  52.00  29.57   50
 55  \w     55.00  80.00   0.50    0.50    --   42.00  52.00  89.81   50
 56  \w     55.00  80.00   0.50    0.50    --   42.00  52.00 -10.47   50
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 62  \w    -89.00 -63.00   0.50    0.50    --  -50.00 -45.00 158.81   52
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 64  \w    -94.00 -68.00   0.50    0.50    --  -54.00 -52.00 134.64   52
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 70  \w    -94.00 -68.00   0.50    0.50    --  -54.00 -52.00 112.95   52
 71  \w    -95.00 -69.00   0.50    0.50    --  -54.00 -52.00 -68.56   52
 72  \w    -93.00 -67.00   0.50    0.50    --  -54.00 -52.00  81.92   52
 73  \w    -94.00 -68.00   0.50    0.50    --  -54.00 -51.00 -40.87   52
 74  \w    -98.00 -72.00   0.50    0.50    --  -58.00 -51.00 -47.42   52
 75  \w    -98.00 -72.00   0.50    0.50    --  -58.00 -52.00 129.26   52
 76  \w    -97.00 -72.00   0.50    0.50    --  -58.00 -49.00  65.05   50
 77  \w    -97.00 -71.00   0.50    0.50    --  -58.00 -52.00-135.68   52
 78  \w    -97.00 -71.00   0.50    0.50    --  -58.00 -51.00-130.24   52
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 80  \w    -99.00 -73.00   0.50    0.50    --  -58.00 -52.00-150.64   52
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 100  \w   -112.00 -86.00   0.50    1.10    --  -74.00 -58.00  55.93   52
 101  \w   -112.00 -86.00   0.50    1.10    --  -74.00 -55.00-177.73   52
 102  \w   -113.00 -87.00   0.50    1.10    --  -74.00 -59.00 -71.46   52
 103  \w   -114.00 -88.00   0.50    1.10    --  -74.00 -55.00-117.89   52
 104  \w   -112.00 -86.00   0.50    1.10    --  -74.00 -58.00 -42.20   52
 105  \w   -112.00 -86.00   0.50    1.10    --  -74.00 -57.00 -78.45   52
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 108  \w   -113.00 -87.00   0.50    1.10    --  -74.00 -60.00 115.17   52
 109  \w   -112.00 -86.00   0.50    1.10    --  -74.00 -56.00-170.23   52
 110  \w   -113.00 -87.00   0.50    1.10    --  -74.00 -58.00  -4.19   52
 111  \w   -114.00 -88.00   0.50    1.10    --  -74.00 -59.00 167.27   52
 112  \w   -112.00 -86.00   0.50    1.10    --  -74.00 -57.00  27.29   52
 113  \w   -113.00 -87.00   0.50    1.10    --  -74.00 -53.00-159.32   52
 114  \w   -116.00 -90.00   0.50    1.10    --  -78.00 -59.00 -23.87   52
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 117  \w   -124.00 -94.00   0.50    1.10    --  -79.50 -64.00 -92.10   60
 118  \w   -117.00 -91.00   0.50    1.10    --  -79.50 -60.00 -43.49   52
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 131  \w   -125.00 -92.00   0.50    1.10    --  -79.50-128.00-176.33   66
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 133  \w   -100.00 -33.00   0.50    1.10    --  -79.50 122.00-173.75  134
 134  \w   -116.00 -90.00   0.50    1.10    --  -79.50 -62.00-134.50   52
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 182  \w     40.00 100.00   0.50    1.10    --   85.25-133.00 130.81  120
 183  \w     99.00 127.00   0.50    1.10    --   85.25 121.00-163.15   56
 184  \w    104.00 132.00   0.50    1.10    --   85.25 113.00  38.51   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
;
 CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      -0.0440209000
_diffrn_orient_matrix_UB_12      0.0519031000
_diffrn_orient_matrix_UB_13      -0.0916669000
_diffrn_orient_matrix_UB_21      -0.0731120000
_diffrn_orient_matrix_UB_22      -0.0729811000
_diffrn_orient_matrix_UB_23      0.0375376000
_diffrn_orient_matrix_UB_31      -0.0759111000
_diffrn_orient_matrix_UB_32      0.0760472000
_diffrn_orient_matrix_UB_33      0.0393310000
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0098
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            123212
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.002
_diffrn_reflns_theta_min         3.057
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    2.176
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.42.57a (Rigaku Oxford Diffraction, 2022) Numerical 
 absorption correction based on gaussian integration over a multifaceted 
 crystal model Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       plate
_exptl_crystal_F_000             1124
_exptl_crystal_preparation
;
 Crystalls were grown from saturated solution of dichloromethane at 23 \%C. 
 For data collection the crystal was immersed in a film of perfluoropolyether 
 oil, mounted on a polyimide loop and transferred to stream of cold nitrogen 
 (Oxford Cryostream 800).
;
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.170
_refine_diff_density_min         -1.228
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         11428
_refine_ls_number_restraints     413
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0805P)^2^+3.2811P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1687
_refine_ls_wR_factor_ref         0.1710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10627
_reflns_number_total             11428
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01814a3.cif
_cod_data_source_block           KR1112_AsSw_a
_cod_depositor_comments
'Adding full bibliography for 1571753--1571754.cif.'
_cod_database_code               1571753
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.722
_shelx_estimated_absorpt_t_max   0.881
_shelx_res_checksum              26111