Synthesis of a Carbon Nanocone by Cascade Annulation.
Shoyama, Kazutaka; Würthner, Frank; Journal of the American Chemical Society 141 (2019) 13008–13012; doi:10.1021/jacs.9b06617

data_4127853
_publ_section_title
;
 Synthesis of a Carbon Nanocone by Cascade Annulation.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13008
_journal_page_last               13012
_journal_paper_doi               10.1021/jacs.9b06617
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C140 H95 N5 O10'
_chemical_formula_sum            'C140 H95 N5 O10'
_chemical_formula_weight         2007.20
_chemical_name_common            C80
_chemical_name_systematic
;
N,N',N'',N''',N''''-pentakis(2,6-diisopropylphenyl)pentanaphtho
[3,4,4a,5,6-bcde:3,4,4a,5,6-ghij:3,4,4a,5,6-lmno:3,4,4a,5,6-
qrst:3,4,4a,5,6-vwxy]circumcorannulene-4,5:8,9:1,20:12,13:16,17-
pentakis(dicarboximide)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 92.015(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0504(10)
_cell_length_b                   23.9374(10)
_cell_length_c                   38.7986(18)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.93
_cell_measurement_theta_min      2.28
_cell_volume                     18610.0(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  Bruker-Kappa-D8Quest_Photon100
_diffrn_measurement_method       omega_and_phi_scan
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1032
_diffrn_reflns_av_unetI/netI     0.1022
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            102415
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.499
_diffrn_reflns_theta_min         2.169
_diffrn_source                   Cu/K(alpha)_ImuS_Microsource
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4200
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1461
_refine_ls_number_reflns         34035
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.1228
_refine_ls_R_factor_gt           0.0857
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1525P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2454
_refine_ls_wR_factor_ref         0.2709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18603
_reflns_number_total             34035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06617_si_002.cif
_cod_data_source_block           c80_tol_sq
_cod_database_code               4127853
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.938
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              46694
_shelx_hkl_checksum              17569
_shelx_fab_checksum              60933