Regioselective Unsymmetrical Tetraallylation of C60 through Palladium Catalysis
Masakazu Nambo; Atsushi Wakamiya; Shigehiro Yamaguchi; Kenichiro Itami; Journal of the American Chemical Society 131 (2009) 15112–15113; doi:10.1021/ja9071173

data_4105215
_publ_contact_author_address
; 
    Department of Chemistry, Graduate School of Science, Nagoya University, 
    Furo, Chikusa, Nagoya 464-8602, Japan
;
_publ_contact_author_email       ' itami@chem.nagoya-u.ac.jp'
_publ_contact_author_fax         ' +81-52-788-6098 '
_publ_contact_author_name        ' Kenichiro Itami '
_publ_contact_author_phone       ' +81-52-788-6098 '
_publ_section_title
;
 Regioselective Unsymmetrical Tetraallylation of C60 through Palladium
 Catalysis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15112
_journal_page_last               15113
_journal_paper_doi               10.1021/ja9071173
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C66 H10'
_chemical_formula_weight         802.74
_chemical_name_common            1,2-diallyl-C60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 109.164(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.505(5)
_cell_length_b                   10.134(3)
_cell_length_c                   20.035(6)
_cell_measurement_reflns_used    7678
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5301
_cell_measurement_theta_min      3.1907
_cell_volume                     3165.4(16)
_computing_molecular_graphics    'ORTEP 3 for windows'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type
;
Saturn70 CCD (4x4 bin mode) with MicroMax-007
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0639
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21546
_diffrn_reflns_theta_full        25.75
_diffrn_reflns_theta_max         25.75
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  0.9952
_exptl_absorpt_correction_T_min  0.9809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_description       plate
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.318
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         5970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.318
_refine_ls_R_factor_all          0.1484
_refine_ls_R_factor_gt           0.1226
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[?^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          0.3440
_refine_ls_wR_factor_ref         0.3630
_reflns_number_gt                3885
_reflns_number_total             5970
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9071173_si_001_2.cif
_cod_data_source_block           comp4
_cod_database_code               4105215