Generation of Fullerenyl Cation (EtO)2P+(OH)CH2-C60+ from RC60-H and from RC60-C60R (R = CH2P(O)(OEt)2)
Yasujiro Murata; Fuyong Cheng; Toshikazu Kitagawa; Koichi Komatsu; Journal of the American Chemical Society 126 (2004) 8874–8875; doi:10.1021/ja047483h

data_4112777
_publ_section_title
;
 Generation of Fullerenyl Cation (EtO)2P+(OH)CH2-C60+ from RC60-H and from
 RC60-C60R (R = CH2P(O)(OEt)2)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8874
_journal_page_last               8875
_journal_paper_doi               10.1021/ja047483h
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C18 H9.5 Br6 F9 N Sb1.5'
_chemical_formula_weight         1072.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                120.000(5)
_cell_formula_units_Z            12
_cell_length_a                   13.533(5)
_cell_length_b                   13.533(5)
_cell_length_c                   51.977(5)
_cell_measurement_temperature    100(2)
_cell_volume                     8244(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1055
_diffrn_reflns_av_sigmaI/netI    0.0739
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            13292
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    10.281
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black_green
_exptl_crystal_density_diffrn    2.593
_exptl_crystal_description       plate
_exptl_crystal_F_000             5904
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.441
_refine_diff_density_min         -1.525
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          4.944
_refine_ls_shift/su_mean         0.045
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1016P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1859
_reflns_number_gt                953
_reflns_number_total             1618
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja047483hsi20040430_015255.cif
_cod_data_source_block           r-3c
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_original_formula_sum        'C18 H9.50 Br6 F9 N Sb1.50'
_cod_database_code               4112777