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_4106175
_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         'C75 H14 S2 '
_chemical_formula_sum            'C75 H14 S2'
_chemical_formula_weight         979.06
_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'
_audit_creation_date             2009-12-10
_audit_creation_method           'by CrystalStructure 3.8'
_cell_angle_alpha                90.0000
_cell_angle_beta                 100.1171(18)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   9.8789(3)
_cell_length_b                   16.4178(5)
_cell_length_c                   24.5759(7)
_cell_measurement_reflns_used    20203
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      3.3
_cell_volume                     3924.0(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    SHELXS97
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.126
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            43936
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    0.829
_exptl_crystal_description       chunk
_exptl_crystal_F_000             992.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.02
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     695
_refine_ls_number_reflns         7154
_refine_ls_R_factor_gt           0.0952
_refine_ls_shift/su_max          0.0020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1987P)^2^+5.1210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.3040
_reflns_number_gt                4942
_reflns_number_total             7154
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja201267t_si_003.cif
_cod_data_source_block           C60Bn2
_cod_original_formula_sum        'C75 H14 S2 '
_cod_database_code               4106175