Synthesis of imino[60]fullerenes using nitriles and trimethylsilylmethyl triflate.
Matsuo, Keiko; Matsuo, Yutaka; Iwashita, Akihiko; Nakamura, Eiichi; Organic letters 11 (2009) 4192–4194; doi:10.1021/ol901851g

data_1504175
_publ_contact_author             'MATSUO, Yutaka'
_publ_section_title
;
 Synthesis of imino[60]fullerenes using nitriles and trimethylsilylmethyl
 triflate.
;
_journal_issue                   18
_journal_name_full               'Organic letters'
_journal_page_first              4192
_journal_page_last               4194
_journal_paper_doi               10.1021/ol901851g
_journal_volume                  11
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C84 H27 Cl2 N1 O1 Si1'
_chemical_formula_sum            'C84 H27 Cl2 N O Si'
_chemical_formula_weight         1165.06
_chemical_name_systematic
;
 ?
;
_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             2009-07-29T19:17:42-00:00
_cell_angle_alpha                90
_cell_angle_beta                 108.3036(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1274(4)
_cell_length_b                   13.9545(3)
_cell_length_c                   19.5256(4)
_cell_measurement_reflns_used    54336
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      68.23
_cell_measurement_theta_min      3.91
_cell_measurement_wavelength     1.5418
_cell_volume                     4947.96(18)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.1312
_diffrn_reflns_av_unetI/netI     0.0885
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54336
_diffrn_reflns_theta_full        68.23
_diffrn_reflns_theta_max         68.23
_diffrn_reflns_theta_min         3.91
_exptl_absorpt_coefficient_mu    1.899
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.387
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         9026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.387
_refine_ls_R_factor_all          0.1666
_refine_ls_R_factor_gt           0.1302
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_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          0.3711
_refine_ls_wR_factor_ref         0.4123
_reflns_number_gt                5238
_reflns_number_total             9026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol901851g_si_002.cif
_cod_data_source_block           iminoAn
_cod_original_cell_volume        4948.0(2)
_cod_database_code               1504175