Sc2@C66 Revisited: An Endohedral Fullerene with Scandium Ions Nestled within Two Unsaturated Linear Triquinanes.
Yamada, Michio; Kurihara, Hiroki; Suzuki, Mitsuaki; Guo, Jing Dong; Waelchli, Markus; Olmstead, Marilyn M.; Balch, Alan L.; Nagase, Shigeru; Maeda, Yutaka; Hasegawa, Tadashi; Lu, Xing; Akasaka, Takeshi; Journal of the American Chemical Society 136 (2014) 7611–7614; doi:10.1021/ja5035649

data_4121831
_publ_section_title
;
 Sc2@C66 Revisited: An Endohedral Fullerene with Scandium Ions Nestled
 within Two Unsaturated Linear Triquinanes.
;
_journal_issue                   21
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7611
_journal_page_last               7614
_journal_paper_doi               10.1021/ja5035649
_journal_volume                  136
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_formula_moiety         4(Sc2C66),1.42(C8H10),1.0(CS2),0.58(C6H14)
_chemical_formula_sum            'C279.84 H22.32 S2 Sc8'
_chemical_formula_weight         3802.70
_chemical_name_common            4(Sc2@C66)/1.42(C8H10)/1.00(CS2)/0.58(C6H14)
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 99.656(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.864(3)
_cell_length_b                   17.514(3)
_cell_length_c                   20.244(3)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    90
_cell_measurement_theta_max      28.65
_cell_measurement_theta_min      2.19
_cell_volume                     6593.5(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.017
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            61844
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.584
_diffrn_reflns_theta_min         1.366
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  0.756
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2012)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.918
_exptl_crystal_description       block
_exptl_crystal_F_000             3803
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.234
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.55(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2681
_refine_ls_number_reflns         36241
_refine_ls_number_restraints     957
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0622
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0810P)^2^+15.3978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.1624
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                33196
_reflns_number_total             36241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5035649_si_002.cif
_cod_data_source_block           Sc2C66
_cod_depositor_comments          'Adding full bibliography for 4121831.cif.'
_cod_original_cell_volume        6593.7(18)
_cod_database_code               4121831
_shelx_estimated_absorpt_t_min   0.881
_shelx_estimated_absorpt_t_max   0.963
_shelxl_version_number           2013-4
_shelx_res_checksum              96509
_shelx_hkl_checksum              90841