Creation of Hoop- and Bowl-Shaped Benzenoid Systems by Selective Detraction of [60]Fullerene Conjugation. [10]Cyclophenacene and Fused Corannulene Derivatives
Yutaka Matsuo; Kazukuni Tahara; Masaya Sawamura; Eiichi Nakamura; Journal of the American Chemical Society 126 (2004) 8725–8734; doi:10.1021/ja048683w

data_4112763
_publ_contact_author             'Nakamura, Eiichi'
_publ_contact_author_email       nakamura@chem.s.u-tokyo.ac.jp
_publ_section_title
;
 Creation of Hoop- and Bowl-Shaped Benzenoid Systems by Selective
 Detraction of [60]Fullerene Conjugation. [10]Cyclophenacene and Fused
 Corannulene Derivatives
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8725
_journal_page_last               8734
_journal_paper_doi               10.1021/ja048683w
_journal_volume                  126
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C104 H66 N1 O3 Rh1'
_chemical_formula_structural     'C104 H66 N1 O3 Rh1'
_chemical_formula_sum            'C104 H66 N O3 Rh'
_chemical_formula_weight         1480.49
_chemical_name_systematic
;
 RhC60Me5CNPh3codTHF3
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3460(7)
_cell_length_b                   14.5830(14)
_cell_length_c                   32.122(3)
_cell_measurement_reflns_used    13000
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.5
_cell_measurement_wavelength     0.71073
_cell_volume                     6720.2(10)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6563
_diffrn_reflns_theta_full        25.74
_diffrn_reflns_theta_max         25.74
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.318
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       prism
_exptl_crystal_F_000             3064
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.033
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.182
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.40(7)
_refine_ls_extinction_coef       0.0066(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         6563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0789
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1342P)^2^+9.4779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1981
_refine_ls_wR_factor_ref         0.2162
_reflns_number_gt                5385
_reflns_number_total             6563
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048683wsi20040514_120946.cif
_cod_data_source_block           Rh[C60(CN)Me5Ph3](cod)
_cod_original_cell_volume        6720.2(9)
_cod_database_code               4112763