Synthesis and Structural, Electrochemical, and Stacking Properties of Conical Molecules Possessing Buckyferrocene on the Apex
Yutaka Matsuo; Ayako Muramatsu; Yuko Kamikawa; Takashi Kato; Eiichi Nakamura; Journal of the American Chemical Society 128 (2006) 9586–9587; doi:10.1021/ja062757h

data_4110771
_publ_contact_author             'NAKAMURA, Eiichi'
_publ_contact_author_email       nakamura@chem.s.u-tokyo.ac.jp
_publ_section_title
;
 Synthesis and Structural, Electrochemical, and Stacking Properties of
 Conical Molecules Possessing Buckyferrocene on the Apex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9586
_journal_page_last               9587
_journal_paper_doi               10.1021/ja062757h
_journal_volume                  128
_journal_year                    2006
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C168 H102 Fe1 O20'
_chemical_formula_sum            'C168 H102 Fe O20'
_chemical_formula_weight         2496.35
_chemical_name_systematic
;
 Fe_C60_C6H4OCOC6H3OR2_5_Cp
;
_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_date             2006-03-16T11:03:10-00:00
_cell_angle_alpha                64.780(5)
_cell_angle_beta                 88.629(5)
_cell_angle_gamma                73.641(5)
_cell_formula_units_Z            2
_cell_length_a                   17.499(5)
_cell_length_b                   18.680(5)
_cell_length_c                   21.896(5)
_cell_measurement_reflns_used    47918
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.75
_cell_measurement_theta_min      2.39
_cell_measurement_wavelength     0.71073
_cell_volume                     6175(3)
_computing_cell_refinement       Scalepack(HKL)
_computing_data_collection       Xpress(MacScience)
_computing_data_reduction        'Denzo and Scalepack(HKL)'
_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      153(2)
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'Imaging Plate'
_diffrn_measurement_method       oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21634
_diffrn_reflns_theta_full        25.75
_diffrn_reflns_theta_max         25.75
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        NA
_diffrn_standards_interval_count NA
_diffrn_standards_number         NA
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       prism
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         4.118
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       0.0153(15)
_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   1.421
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1563
_refine_ls_number_reflns         21634
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.421
_refine_ls_R_factor_all          0.1427
_refine_ls_R_factor_gt           0.1139
_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          0.329
_refine_ls_wR_factor_ref         0.3584
_reflns_number_gt                15341
_reflns_number_total             21634
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja062757hsi20060420_085839.cif
_cod_data_source_block           FeC1
_cod_database_code               4110771