Reversible σ-Bond Formation in Bowl-Shaped π-Radical Cations: The Effects of Curved and Planar Structures.
Yokoi, Hiroki; Hiroto, Satoru; Shinokubo, Hiroshi; Journal of the American Chemical Society 140 (2018) 4649–4655; doi:10.1021/jacs.8b00798

data_4132040
_publ_section_title
;
 Reversible \s-Bond Formation in Bowl-Shaped \p-Radical Cations: The
 Effects of Curved and Planar Structures.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4649
_journal_page_last               4655
_journal_paper_doi               10.1021/jacs.8b00798
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C128.76 H137.19 Cl14.9 N2 O2.73 Sb2'
_chemical_formula_weight         2528.09
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.309(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.3774(8)
_cell_length_b                   12.2907(3)
_cell_length_c                   29.9008(7)
_cell_measurement_reflns_used    11220
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      25.3480
_cell_measurement_theta_min      1.8350
_cell_volume                     11898.6(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0811
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            72103
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.772
_exptl_absorpt_coefficient_mu    0.842
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5204
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.124
_refine_diff_density_max         1.689
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     836
_refine_ls_number_reflns         10424
_refine_ls_number_restraints     256
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+61.6386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1430
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8781
_reflns_number_total             10424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b00798_si_004.cif
_cod_data_source_block           yokoi170820d8_a
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C128.76 H137.19 Cl14.90 N2 O2.73 Sb2'
_cod_database_code               4132040
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.773
_shelx_estimated_absorpt_t_max   0.903
_shelx_res_checksum              16555
_shelx_hkl_checksum              52253