Formation of Singly Bonded PhCH2C60-C60CH2Ph Dimers from 1,2-(PhCH2)HC60 via Electroreductive C60-H Activation
Wei-Wei Yang; Zong-Jun Li; Xiang Gao; Journal of Organic Chemistry 76 (2011) 6067–6074; doi:10.1021/jo2006768

data_4026477
_publ_section_title
;
 Formation of Singly Bonded PhCH2C60-C60CH2Ph Dimers from 1,2-(PhCH2)HC60
 via Electroreductive C60-H Activation
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6067
_journal_page_last               6074
_journal_paper_doi               10.1021/jo2006768
_journal_volume                  76
_journal_year                    2011
_chemical_formula_sum            'C176 H56'
_chemical_formula_weight         2170.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.398(1)
_cell_angle_beta                 91.499(1)
_cell_angle_gamma                115.592(1)
_cell_formula_units_Z            1
_cell_length_a                   13.2330(7)
_cell_length_b                   14.1032(8)
_cell_length_c                   14.6106(8)
_cell_measurement_reflns_used    5789
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      26.03
_cell_measurement_theta_min      2.18
_cell_volume                     2402.1(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      143(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII 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     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17255
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.9915
_exptl_absorpt_correction_T_min  0.9789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       prism
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     991
_refine_ls_number_reflns         8439
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1449
_refine_ls_R_factor_gt           0.0974
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1191P)^2^+4.9711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2508
_refine_ls_wR_factor_ref         0.2851
_reflns_number_gt                5272
_reflns_number_total             8439
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo2006768_si_002.cif
_cod_data_source_block           gao3
_cod_database_code               4026477