Electrochemical reduction of cationic Li+@C60to neutral Li+@C60˙−: isolation and characterisation of endohedral [60]fulleride
Ueno, Hiroshi; Aoyagi, Shinobu; Yamazaki, Yu; Ohkubo, Kei; Ikuma, Naohiko; Okada, Hiroshi; Kato, Tatsuhisa; Matsuo, Yutaka; Fukuzumi, Shunichi; Kokubo, Ken; Chem. Sci. 7 (2016) 5770–; doi:10.1039/C6SC01209D

data_1543493
_publ_section_title
;
 Electrochemical reduction of cationic Li+@C60to neutral
 Li+@C60&#x02D9;&#x2212;: isolation and characterisation of endohedral
 [60]fulleride
;
_journal_issue                   9
_journal_name_full               'Chem. Sci.'
_journal_page_first              5770
_journal_paper_doi               10.1039/C6SC01209D
_journal_volume                  7
_journal_year                    2016
_chemical_formula_sum            'C194 H92 Cl4 Li2 N8 Ni2'
_chemical_formula_weight         2807.9
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-03-07 deposited with the CCDC.
2016-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.543(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.4000(10)
_cell_length_b                   14.8640(10)
_cell_length_c                   17.2330(10)
_cell_measurement_reflns_used    3838
_cell_measurement_temperature    100
_cell_measurement_theta_max      18.517
_cell_measurement_theta_min      0.946
_cell_volume                     5925.6(6)
_computing_cell_refinement       'RAPID-AUTO (Rigaku Corporation)'
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation)'
_computing_data_reduction        'RAPID-AUTO (Rigaku Corporation)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_device_type  'Large cylindrical imaging plate camera'
_diffrn_measurement_method       'Oscilation method'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41286
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51476
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        14.343
_diffrn_reflns_theta_max         18.517
_diffrn_reflns_theta_min         0.946
_diffrn_source                   'SPring-8 BL02B1 bending magnet'
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       plate
_exptl_crystal_F_000             2884
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1003
_refine_ls_number_reflns         10513
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1550
_refine_ls_wR_factor_ref         0.1569
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10306
_reflns_number_total             10513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc01209d2.cif
_cod_data_source_block           LiC60-NiOEP_100K
_cod_depositor_comments
'Adding full bibliography for 1543493--1543494.cif.'
_cod_database_code               1543493
_shelxl_version_number           2013-2
_shelx_res_checksum              83765
_shelx_hkl_checksum              76868