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_4112762
_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         'C105 H50 Cl1 N1 Pd1'
_chemical_formula_structural     'C105 H50 Cl1 N1 Pd1'
_chemical_formula_sum            'C105 H50 Cl N Pd'
_chemical_formula_weight         1467.31
_chemical_name_systematic
;
 Pd-allyl-C60Ph5Me5CN
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90
_cell_angle_beta                 97.044(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.9920(17)
_cell_length_b                   27.547(2)
_cell_length_c                   32.7300(14)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     13415.0(19)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.856
_diffrn_measured_fraction_theta_max 0.856
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0926
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            21958
_diffrn_reflns_theta_full        25.75
_diffrn_reflns_theta_max         25.75
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       prism
_exptl_crystal_F_000             6000
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.696
_refine_diff_density_min         -1.773
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       0.0017(2)
_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   0.993
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1944
_refine_ls_number_reflns         21958
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1801
_refine_ls_R_factor_gt           0.1054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2705
_refine_ls_wR_factor_ref         0.324
_reflns_number_gt                9462
_reflns_number_total             21958
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048683wsi20040514_120922.cif
_cod_data_source_block           Pd[C60(CN)Me5Ph5](allyl)
_cod_original_cell_volume        13415(2)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4112762