Stable cationic nanobelts synthesized by chemical oxidation of methylene-bridged [6]cycloparaphenylene
Kai, Nobushige; Kono, Hideya; Stünkel, Timo; Imoto, Daiki; Zanasi, Riccardo; Monaco, Guglielmo; Summa, Francesco F.; Scott, Lawrence T.; Yagi, Akiko; Itami, Kenichiro; Chemical Science 16 (2025) 9195–9202; doi:10.1039/D5SC01305D

data_1574486
_publ_section_title
;
 Stable cationic nanobelts synthesized by chemical oxidation of
 methylene-bridged [6]cycloparaphenylene
;
_journal_issue                   21
_journal_name_full               'Chemical Science'
_journal_page_first              9195
_journal_page_last               9202
_journal_paper_doi               10.1039/D5SC01305D
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         '2(F6 Sb), 5(C H2 Cl2), C42 H24'
_chemical_formula_sum            'C47 H34 Cl10 F12 Sb2'
_chemical_formula_weight         1424.74
_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
_audit_creation_date             2023-10-16
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2018.12.05 svn.r3537 for Rigaku Oxford Diffraction, GUI svn.r5625)
;
_audit_update_record
;
2024-05-30 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                105.769(2)
_cell_angle_beta                 104.054(2)
_cell_angle_gamma                116.448(2)
_cell_formula_units_Z            1
_cell_length_a                   11.0560(3)
_cell_length_b                   12.0361(2)
_cell_length_c                   12.1017(3)
_cell_measurement_reflns_used    15461
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.1280
_cell_measurement_theta_min      2.0660
_cell_volume                     1257.78(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.821
_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    -67.00  13.00   0.50   10.00    --    3.32 -62.00 -16.00  160
  2  \w     27.00  72.00   0.50   10.00    --    3.32  62.00 122.00   90
  3  \w    -19.00  30.00   0.50   10.00    --   -2.70  57.00-120.00   98
  4  \w    -17.00  77.00   0.50   10.00    --   -2.70  19.00 120.00  188
  5  \w     -6.00  38.00   0.50   10.00    --    3.32 -99.00-120.00   88
  6  \w    -11.00  14.00   0.50   10.00    --    3.32 -99.00 120.00   50
  7  \w    -12.00  37.00   0.50   10.00    --    3.32 -99.00 -30.00   98
  8  \w    -11.00  36.00   0.50   10.00    --    3.32 -99.00  60.00   94
  9  \w      8.00  33.00   0.50   10.00    --    3.32 -99.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0651557000
_diffrn_orient_matrix_UB_12      -0.0016870000
_diffrn_orient_matrix_UB_13      -0.0290724000
_diffrn_orient_matrix_UB_21      -0.0377379000
_diffrn_orient_matrix_UB_22      -0.0716765000
_diffrn_orient_matrix_UB_23      -0.0388761000
_diffrn_orient_matrix_UB_31      -0.0240735000
_diffrn_orient_matrix_UB_32      -0.0147319000
_diffrn_orient_matrix_UB_33      0.0464526000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.821
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19722
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.921
_diffrn_reflns_theta_min         1.929
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.685
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_description       plate
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.006
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5972
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0259
_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^)+(0.0295P)^2^+1.2796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0639
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5528
_reflns_number_total             5972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01305d2.cif
_cod_data_source_block           kai316a_6mcppcation_ch2cl2_auto
_cod_depositor_comments          'Adding full bibliography for 1574486.cif.'
_cod_original_cell_volume        1257.78(6)
_cod_database_code               1574486
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H Sb F Cl '
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.751
_diffrn_oxdiff_digest_frames
;
010980833ad92e22a1943d2d3712b2691500025b6e8
;
_diffrn_oxdiff_digest_hkl
;
010cb771c33b3ba8a5aff1190c4d191e8df3ce
;
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl33-C32 = Cl34-C32
 1.76 with sigma of 0.01
3. Others
 Fixed Sof: Cl34(0.5) Cl33(0.5) C32(0.5) H2A(0.5) H2B(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C6(H00A,H00B), C1(H00C,H00D), C16(H00E,H00F), C35(H00G,H00K), C29(H01A,H01B),
 C32(H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 C18(H00H), C4(H00I), C8(H00J), C11(H00N), C21(H00Q), C14(H00R)
;
_shelx_res_checksum              11369
_shelx_hkl_checksum              56612
_olex2_exptl_crystal_mounting_method loop
_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 1.720
_oxdiff_exptl_absorpt_empirical_full_min 0.608