Cu(i)-mediated regioselective tri-addition of Grignard reagent to [70]fullerene. Synthesis of indenyl-type metal ligand embedded into graphitic structure
Sawamura, Masaya; Toganoh, Motoki; Iikura, Hitoshi; Matsuo, Yutaka; Hirai, Atsushi; Nakamura, Eiichi; Journal of Materials Chemistry 12 (2002) 2109–; doi:10.1039/b202130g

data_7204382
_publ_contact_author             'Prof Eiichi Nakamura'
_publ_section_title
;
 Cu(i)-mediated regioselective tri-addition of Grignard reagent to
 [70]fullerene. Synthesis of indenyl-type metal ligand embedded into
 graphitic structure
;
_journal_issue                   7
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              2109
_journal_paper_doi               10.1039/b202130g
_journal_volume                  12
_journal_year                    2002
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C103 H20 Cl4 F9 Tl1'
_chemical_formula_structural     'C103 H20 Cl4 F9 TL1'
_chemical_formula_sum            'C103 H20 Cl4 F9 Tl'
_chemical_formula_weight         1774.36
_chemical_name_common            C70Ar3Tl
_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
_audit_creation_date             2002-01-23T02:05:58-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90.000
_cell_angle_beta                 109.861(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   18.419(5)
_cell_length_b                   17.565(5)
_cell_length_c                   20.638(5)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71069
_cell_volume                     6280(3)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.473
_diffrn_measured_fraction_theta_max 0.473
_diffrn_measurement_device_type  MacScienceDIP2030
_diffrn_measurement_method       scanning
_diffrn_radiation_detector       'Imaging Plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_unetI/netI     0.1645
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5791
_diffrn_reflns_theta_full        25.91
_diffrn_reflns_theta_max         25.91
_diffrn_reflns_theta_min         4.32
_exptl_absorpt_coefficient_mu    2.833
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.877
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3472
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.317
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         5791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.2232
_refine_ls_R_factor_gt           0.0972
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[&#x00AB;s^2^(Fo^2^)+(0.1515P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2408
_refine_ls_wR_factor_ref         0.3192
_reflns_number_gt                2323
_reflns_number_total             5791
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b202130g.txt
_cod_data_source_block           C70Ar3Tl
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7204382