Protonated [4n]π and [4n+2]π Octaphyrins Choose Their Möbius/Hückel Aromatic Topology
Jong Min Lim; Jae-Yoon Shin; Yasuo Tanaka; Shohei Saito; Atsuhiro Osuka; Dongho Kim; Journal of the American Chemical Society 132 (2010) 3105–3114; doi:10.1021/ja909744z

data_4102008
_publ_section_title
;
 Protonated [4n]\p and [4n+2]\p Octaphyrins Choose Their M\"obius/H\"uckel
 Aromatic Topology
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3105
_journal_page_last               3114
_journal_paper_doi               10.1021/ja909744z
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C88 H22 F40 N8, 2(C2 F3 O2), 6(C2 H F3 O2)'
_chemical_formula_sum            'C104 H28 F64 N8 O16'
_chemical_formula_weight         2861.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 104.353(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.357(2)
_cell_length_b                   22.0294(16)
_cell_length_c                   38.924(4)
_cell_measurement_reflns_used    5692
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      22.20
_cell_measurement_theta_min      2.31
_cell_volume                     25218(4)
_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      90(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0820
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            64857
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    0.165
_exptl_absorpt_correction_T_max  0.9523
_exptl_absorpt_correction_T_min  0.9223
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             11296
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_platon_squeeze_details
;
;
_refine_diff_density_max         1.668
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1729
_refine_ls_number_reflns         22159
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1390
_refine_ls_R_factor_gt           0.0939
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1755P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2698
_refine_ls_wR_factor_ref         0.2905
_reflns_number_gt                12196
_reflns_number_total             22159
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja909744z_si_001.cif
_cod_data_source_block           80419sa
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4102008