A triply linked propellane-nanoring hybrid serving as a good host
Chen, Yan; Chen, Xingyu; Li, Lin; Chen, Xiangping; Xia, Jianlong; Zhang, Lei; Chemical Science 16 (2025) 6822–6827; doi:10.1039/D5SC00713E

data_1574138
_publ_section_title
;
 A triply linked propellane-nanoring hybrid serving as a good host
;
_journal_issue                   16
_journal_name_full               'Chemical Science'
_journal_page_first              6822
_journal_page_last               6827
_journal_paper_doi               10.1039/D5SC00713E
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         '4(C H Cl3), C78 H84'
_chemical_formula_sum            'C82 H88 Cl12'
_chemical_formula_weight         1498.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-01-13 deposited with the CCDC.	2025-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.8490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4184(2)
_cell_length_b                   29.5605(4)
_cell_length_c                   16.8961(2)
_cell_measurement_reflns_used    12931
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      75.9360
_cell_measurement_theta_min      2.9910
_cell_volume                     8025.56(18)
_computing_cell_refinement       'CrysAlisPro 1.171.43.114a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.114a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.114a (Rigaku OD, 2024)'
_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      170.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.956
_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    -22.00  26.00   0.50    0.80    --  -46.59  77.00  -2.00   96
  2  \w    -53.00 -27.00   0.50    0.80    --  -46.59  77.00  -2.00   52
  3  \w    -25.00  55.00   0.50    0.80    --   46.59 -77.00-128.00  160
  4  \w     47.00  72.00   0.50    0.80    --   46.59  77.00  -2.00   50
  5  \w    -84.00 -47.00   0.50    2.00    -- -103.72  77.00  -2.00   74
  6  \w   -168.00-142.00   0.50    2.00    -- -103.72 -77.00-128.00   52
  7  \w   -141.00 -81.00   0.50    2.00    -- -103.72 -77.00-128.00  120
  8  \w     53.00 106.00   0.50    2.00    --  103.72 -77.00-128.00  106
  9  \w   -102.00 -47.00   0.50    0.80    --  -46.59 -77.00-128.00  110
 10  \w    -20.00  28.00   0.50    0.80    --  -46.59  19.00   0.00   96
 11  \w     -2.00  28.00   0.50    0.80    --  -46.59  19.00 150.00   60
 12  \w    -62.00 -34.00   0.50    2.00    -- -103.72  61.00 150.00   56
 13  \w    -68.00 -34.00   0.50    2.00    -- -103.72  61.00 -60.00   68
 14  \w    -68.00 -31.00   0.50    2.00    -- -103.72  61.00  60.00   74
 15  \w   -120.00 -93.00   0.50    2.00    -- -103.72 -45.00 -60.00   54
 16  \w    -67.00 -31.00   0.50    2.00    -- -103.72  61.00 -90.00   72
 17  \w    -56.00 -31.00   0.50    2.00    -- -103.72  61.00-150.00   50
 18  \w   -101.00 -31.00   0.50    2.00    -- -103.72  77.00-180.00  140
 19  \w   -171.00-126.00   0.50    2.00    -- -103.72 -45.00 -60.00   90
 20  \w    -68.00 -31.00   0.50    2.00    -- -103.72  61.00   0.00   74
 21  \w     31.00  74.00   0.50    2.00    --  103.72 -61.00   0.00   86
 22  \w     46.00  74.00   0.50    2.00    --  103.72 -61.00  30.00   56
 23  \w     92.00 156.00   0.50    2.00    --  103.72  15.00 -60.00  128
 24  \w     42.00  71.00   0.50    2.00    --  103.72 -61.00  60.00   58
 25  \w     93.00 175.00   0.50    2.00    --  103.72  45.00 -60.00  164
 26  \w    104.00 129.00   0.50    2.00    --  103.72  77.00  -2.00   50
;
_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      0.0092221000
_diffrn_orient_matrix_UB_12      0.0183964000
_diffrn_orient_matrix_UB_13      -0.0830104000
_diffrn_orient_matrix_UB_21      0.0588796000
_diffrn_orient_matrix_UB_22      -0.0394549000
_diffrn_orient_matrix_UB_23      -0.0086752000
_diffrn_orient_matrix_UB_31      -0.0750973000
_diffrn_orient_matrix_UB_32      -0.0286447000
_diffrn_orient_matrix_UB_33      -0.0414179000
_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  0.0330
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29421
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.152
_diffrn_reflns_theta_min         2.990
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.102
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.114a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_description       prism
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.189
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         8051
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0813
_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^)+(0.1278P)^2^+22.0047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2260
_refine_ls_wR_factor_ref         0.2358
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6721
_reflns_number_total             8051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00713e2.cif
_cod_data_source_block           fx527_auto
_cod_depositor_comments
'Adding full bibliography for 1574137--1574139.cif.'
_cod_database_code               1574138
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CH
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C29 \\sim C30 \\sim C31 \\sim C32 \\sim C30A \\sim C31A \\sim C32A: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
C33 \\sim C34 \\sim C35 \\sim C36 \\sim C34A \\sim C35A \\sim C36A: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
Uanis(C32A) \\sim Ueq, Uanis(C36A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31A)=Sof(H31D)=Sof(H31E)=
 Sof(H31F)=Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(1)
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(1)
 Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35A)=Sof(H35D)=Sof(H35E)=
 Sof(H35F)=Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(2)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=
 Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(2)
 Sof(C42A)=Sof(H42A)=1-FVAR(3)
 Sof(C42)=Sof(H42)=FVAR(3)
4.a Ternary CH refined with riding coordinates:
 C41(H41), C42(H42), C42A(H42A)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C8(H8), C9(H9), C10(H10), C12(H12), C14(H14),
 C16(H16), C18(H18), C20(H20), C22(H22), C24(H24), C26(H26), C27(H27), C28(H28)
4.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C30A(H30D,H30E,H30F), C31A(H31D,H31E,H31F),
 C32A(H32D,H32E,H32F), C34A(H34D,H34E,H34F), C35A(H35D,H35E,H35F), C36A(H36D,
 H36E,H36F)
;
_shelx_res_checksum              26020
_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 2.082
_oxdiff_exptl_absorpt_empirical_full_min 0.490