Aromatic π-Systems More Curved Than C60. The Complete Family of All Indenocorannulenes Synthesized by Iterative Microwave-Assisted Intramolecular Arylations
Brian D. Steinberg; Edward A. Jackson; Alexander S. Filatov; Atsushi Wakamiya; Marina A. Petrukhina; Lawrence T. Scott; Journal of the American Chemical Society 131 (2009) 10537–10545; doi:10.1021/ja9031852

data_4104762
_publ_contact_author_address
;
Merkert Chemistry Center
Department of Chemistry
Boston College
Chestnut Hill
Massachusetts 02467-3860
USA
;
_publ_contact_author_email       lawrence.scott@bc.edu
_publ_contact_author_fax         617-552-6454
_publ_contact_author_name
;
Scott, Lawrence T. 
;
_publ_contact_author_phone       617-552-8024
_publ_section_title
;
 Aromatic \p-Systems More Curved Than C60. The Complete Family of All
 Indenocorannulenes Synthesized by Iterative Microwave-Assisted
 Intramolecular Arylations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10537
_journal_page_last               10545
_journal_paper_doi               10.1021/ja9031852
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C38.25 H16 S0.5'
_chemical_formula_weight         491.54
_chemical_name_systematic
; 
 triindeno[1,2,3-bc:1',2',3'-ef:1'',2'',3''-hi]corannulene 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.367(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.578(4)
_cell_length_b                   4.0865(6)
_cell_length_c                   42.620(7)
_cell_measurement_reflns_used    2820
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      22.06
_cell_measurement_theta_min      2.28
_cell_volume                     4367.5(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0680
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            30480
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         0.86
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_meas      0
_exptl_crystal_description       sliver
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     700
_refine_ls_number_reflns         10932
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0857P)^2^+1.2043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1834
_reflns_number_gt                6952
_reflns_number_total             10932
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9031852_si_001_5.cif
_cod_data_source_block           1,2,3-tri-IC
_cod_original_cell_volume        4367.6(11)
_cod_original_formula_sum        'C38.25 H16 S0.50'
_cod_database_code               4104762