Covalently chemical modification of lithium ion-encapsulated fullerene: synthesis and characterization of [Li+@PCBM]PF6(-).
Matsuo, Yutaka; Okada, Hiroshi; Maruyama, Masashi; Sato, Hiroyasu; Tobita, Hiromi; Ono, Yoshihiro; Omote, Kenji; Kawachi, Kazuhiko; Kasama, Yasuhiko; Organic letters 14 (2012) 3784–3787; doi:10.1021/ol301671n

data_1508320
_publ_section_title
;
 Covalently chemical modification of lithium ion-encapsulated fullerene:
 synthesis and characterization of [Li+@PCBM]PF6(-).
;
_journal_issue                   14
_journal_name_full               'Organic letters'
_journal_page_first              3784
_journal_page_last               3787
_journal_paper_doi               10.1021/ol301671n
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C73 H16 Cl2 F6 Li O2 P'
_chemical_formula_sum            'C73 H16 Cl2 F6 Li O2 P'
_chemical_formula_weight         1147.74
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 99.567(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   9.8919(13)
_cell_length_b                   19.910(3)
_cell_length_c                   21.435(3)
_cell_measurement_reflns_used    6433
_cell_measurement_temperature    93
_cell_measurement_theta_max      65.46
_cell_measurement_theta_min      3.05
_cell_volume                     4162.9(10)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXD (Schneider, et al., 2002)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1715
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_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            18890
_diffrn_reflns_theta_full        40.00
_diffrn_reflns_theta_max         40.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.551
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2304.00
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.810
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     236
_refine_ls_number_reflns         2532
_refine_ls_number_restraints     237
_refine_ls_R_factor_gt           0.2449
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'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_ref         0.5918
_reflns_number_gt                1555
_reflns_number_total             2532
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol301671n_si_002.cif
_cod_data_source_block           66LiPCBM
_cod_depositor_comments
;

    Adding full bibliography for 1508320.cif.

    Marking alternative atoms according to the Supporting Information of
    the original publication: atoms with occupancy value of '0.72(4)' are
    assigned to group 1 of assembly A and atoms with occupancy value of
    '0.28(4)' are assigned to group 2 of assembly A.

    Andrius Merkys
    2014-08-29

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_cod_database_code               1508320