A Scalable Synthesis of Methano[60]fullerene and Congeners by the Oxidative Cyclopropanation Reaction of Silylmethylfullerene
Ying Zhang; Yutaka Matsuo; Chang-Zhi Li; Hideyuki Tanaka; Eiichi Nakamura; Journal of the American Chemical Society 133 (2011) 8086–8089; doi:10.1021/ja201267t

data_4106174
_publ_contact_author_email       matsuo@chem.s.u-tokyo.ac.jp
_publ_contact_author_fax         +81-3-5841-1476
_publ_contact_author_name        'MATSUO, Yutaka'
_publ_contact_author_phone       +81-3-5841-1476
_publ_section_title
;
 A Scalable Synthesis of Methano[60]fullerene and Congeners by the
 Oxidative Cyclopropanation Reaction of Silylmethylfullerene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8086
_journal_page_last               8089
_journal_paper_doi               10.1021/ja201267t
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C76 H17 Cl3 '
_chemical_formula_sum            'C76 H17 Cl3'
_chemical_formula_weight         1036.33
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             2009-12-03
_audit_creation_method           'by CrystalStructure 3.8'
_cell_angle_alpha                90.0000
_cell_angle_beta                 101.6438(17)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   9.9678(3)
_cell_length_b                   22.5433(7)
_cell_length_c                   20.4289(6)
_cell_measurement_reflns_used    27814
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      68.3
_cell_measurement_theta_min      3.0
_cell_volume                     4496.1(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR88
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.110
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            52044
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_exptl_absorpt_coefficient_mu    1.137
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    0.765
_exptl_crystal_description       block
_exptl_crystal_F_000             1048.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.90
_refine_diff_density_min         -1.27
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.994
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     749
_refine_ls_number_reflns         8200
_refine_ls_R_factor_gt           0.1618
_refine_ls_shift/su_max          0.01
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.4554
_reflns_number_gt                6441
_reflns_number_total             8200
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja201267t_si_002.cif
_cod_data_source_block           C61H2Bn2
_cod_original_cell_volume        4496.0(2)
_cod_original_formula_sum        'C76 H17 Cl3 '
_cod_database_code               4106174