Buckybowl and its chiral hybrids featuring eight-membered rings and helicene units.
Duan, Yuxiao; Chen, Meng; Hayashi, Hironobu; Yamada, Hiroko; Liu, Xinyue; Zhang, Lei; Chemical science 14 (2023) 10420–10428; doi:10.1039/d3sc00658a

data_1568664
_publ_section_title
;
 Buckybowl and its chiral hybrids featuring eight-membered rings and
 helicene units.
;
_journal_issue                   38
_journal_name_full               'Chemical science'
_journal_page_first              10420
_journal_page_last               10428
_journal_paper_doi               10.1039/d3sc00658a
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C72 H56 Cl2, C H Cl3'
_chemical_formula_sum            'C73 H57 Cl5'
_chemical_formula_weight         1111.43
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-03
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-09-05 deposited with the CCDC.	2023-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   31.90908(14)
_cell_length_b                   31.90908(14)
_cell_length_c                   37.27060(18)
_cell_measurement_reflns_used    54468
_cell_measurement_temperature    169.99(12)
_cell_measurement_theta_max      75.0010
_cell_measurement_theta_min      2.7480
_cell_volume                     32864.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(12)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_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    -48.00  24.00   0.50    0.30    --  -47.57  46.00  19.00  144
  2  \w   -118.00 -35.00   0.50    0.30    --  -47.57 -46.00-130.00  166
  3  \w     62.00  88.00   0.50    0.30    --   47.57  46.00  19.00   52
  4  \w     -7.00  37.00   0.50    0.30    --   47.57 -46.00-130.00   88
  5  \w   -151.00-126.00   0.50    1.50    --  -99.00 -46.00-130.00   50
  6  \w     91.00 168.00   0.50    1.50    --  103.25  46.00  19.00  154
  7  \w   -116.00 -84.00   0.50    0.30    --  -47.57-125.00   0.00   64
  8  \w    -19.00  17.00   0.50    0.30    --  -47.57  19.00-180.00   72
  9  \w    -55.00 -29.00   0.50    1.50    --  -99.00  61.00-180.00   52
 10  \w   -148.00 -98.00   0.50    1.50    --  -99.00 -45.00 -60.00  100
 11  \w    -68.00 -27.00   0.50    1.50    --  -99.00  61.00 -60.00   82
 12  \w    -66.00 -27.00   0.50    1.50    --  -99.00  61.00-120.00   78
 13  \w    -63.00 -27.00   0.50    1.50    --  -99.00  61.00 -90.00   72
 14  \w    -62.00 -31.00   0.50    1.50    --  -99.00  61.00   0.00   62
 15  \w    -97.00 -38.00   0.50    1.50    --  -99.00  77.00 150.00  118
 16  \w     39.00  65.00   0.50    1.50    --  103.25 -61.00  90.00   52
 17  \w    116.00 164.00   0.50    1.50    --  103.25  30.00 -30.00   96
 18  \w     88.00 143.00   0.50    1.50    --  103.25 125.00-150.00  110
 19  \w     42.00  75.00   0.50    1.50    --  103.25 -61.00   0.00   66
 20  \w     45.00  72.00   0.50    1.50    --  103.25 -61.00 -60.00   54
 21  \w    143.00 169.00   0.50    1.50    --  103.25  45.00 -60.00   52
 22  \w     91.00 130.00   0.50    1.50    --  103.25  45.00 -60.00   78
 23  \w    107.00 167.00   0.50    1.50    --  103.25  30.00 120.00  120
 24  \w     32.00  75.00   0.50    1.50    --  103.25 -61.00  30.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0004049000
_diffrn_orient_matrix_UB_12      0.0320929000
_diffrn_orient_matrix_UB_13      0.0310356000
_diffrn_orient_matrix_UB_21      0.0065977000
_diffrn_orient_matrix_UB_22      -0.0327298000
_diffrn_orient_matrix_UB_23      0.0270730000
_diffrn_orient_matrix_UB_31      0.0553559000
_diffrn_orient_matrix_UB_32      0.0317391000
_diffrn_orient_matrix_UB_33      -0.0034525000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            77970
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.283
_diffrn_reflns_theta_min         2.770
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.070
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.011
_exptl_crystal_description       block
_exptl_crystal_F_000             10440
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.574
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         14721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1027P)^2^+77.4585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1845
_refine_ls_wR_factor_ref         0.1871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13605
_reflns_number_total             14721
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00658a2.cif
_cod_data_source_block           tx9629_sq
_cod_depositor_comments
'Adding full bibliography for 1568662--1568666.cif.'
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               1568664
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHCl
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C73(H73)
1.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C9(H9), C10(H10), C11(H11), C12(H12), C17(H17), C18(H18),
 C20(H20), C23(H23), C25(H25), C28(H28), C30(H30), C33(H33), C35(H35), C36(H36),
  C41(H41), C42(H42), C43(H43), C44(H44)
1.c Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,
 H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C), C67(H67A,
 H67B,H67C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C),
 C72(H72A,H72B,H72C)
;
_shelx_res_checksum              104
_shelx_fab_checksum              3080
_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 1.775
_oxdiff_exptl_absorpt_empirical_full_min 0.581