Facile Formation of a Benzopyrane-Fused [28]Hexaphyrin That Exhibits Distinct Möbius Aromaticity
Sumito Tokuji; Jae-Yoon Shin; Kil Suk Kim; Jong Min Lim; Katsuyuki Youfu; Shohei Saito; Dongho Kim; Atsuhiro Osuka; Journal of the American Chemical Society 131 (2009) 7240–7241; doi:10.1021/ja902836x

data_4104466
_publ_section_title
;
 Facile Formation of a Benzopyrane-Fused [28]Hexaphyrin That Exhibits
 Distinct M\"obius Aromaticity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7240
_journal_page_last               7241
_journal_paper_doi               10.1021/ja902836x
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C66 H15 F29 N6 O, C6 H14'
_chemical_formula_sum            'C72 H29 F29 N6 O'
_chemical_formula_weight         1545.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.79(7)
_cell_angle_beta                 88.10(9)
_cell_angle_gamma                67.33(9)
_cell_formula_units_Z            2
_cell_length_a                   14.19(3)
_cell_length_b                   14.83(3)
_cell_length_c                   17.49(4)
_cell_measurement_reflns_used    16258
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     3210(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_sigmaI/netI    0.0819
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19367
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    0.155
_exptl_absorpt_correction_T_max  0.9696
_exptl_absorpt_correction_T_min  0.8992
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       prism
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     975
_refine_ls_number_reflns         9601
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1401
_refine_ls_R_factor_gt           0.1057
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1527P)^2^+5.3122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2693
_refine_ls_wR_factor_ref         0.3035
_reflns_number_gt                5957
_reflns_number_total             9601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja902836x_si_002.cif
_cod_data_source_block           hexa_o
_cod_original_cell_volume        3211(13)
_cod_database_code               4104466