Crystallographic Structure Determination of Both [5,6]- and [6,6]-Isomers of Lithium-Ion-Containing Diphenylmethano[60]fullerene.
Okada, Hiroshi; Kawakami, Hiroki; Aoyagi, Shinobu; Matsuo, Yutaka; The Journal of organic chemistry 82 (2017) 5868–5872; doi:10.1021/acs.joc.7b00730

data_4032551
_publ_section_title
;
 Crystallographic Structure Determination of Both [5,6]- and [6,6]-Isomers
 of Lithium-Ion-Containing Diphenylmethano[60]fullerene.
;
_journal_issue                   11
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5868
_journal_page_last               5872
_journal_paper_doi               10.1021/acs.joc.7b00730
_journal_volume                  82
_journal_year                    2017
_chemical_formula_sum            'C79.63 H13.86 Cl0.77 F6 Li N O4 S2'
_chemical_formula_weight         1260.67
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                85.740(10)
_cell_angle_beta                 72.950(10)
_cell_angle_gamma                68.680(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3770(10)
_cell_length_b                   14.5170(10)
_cell_length_c                   18.313(2)
_cell_measurement_reflns_used    1151
_cell_measurement_temperature    100
_cell_measurement_theta_max      14.96
_cell_measurement_theta_min      1.0
_cell_volume                     2455.4(5)
_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 0.907
_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     0.41289
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.3184
_diffrn_reflns_Laue_measured_fraction_full 0.907
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14255
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        14.343
_diffrn_reflns_theta_max         14.950
_diffrn_reflns_theta_min         1.125
_diffrn_source                   'SPring-8 BL02B1 bending magnet'
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             1265.4
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1107
_refine_ls_number_reflns         5287
_refine_ls_number_restraints     2743
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0653
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1300P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1823
_refine_ls_wR_factor_ref         0.1833
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5178
_reflns_number_total             5287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b00730_si_001.cif
_cod_data_source_block           56-LiC61Ph2_TFSI_C6H5Cl
_cod_original_cell_volume        2455.4(4)
_cod_database_code               4032551
_shelxl_version_number           2013-2
_shelx_res_checksum              6698
_shelx_hkl_checksum              84748