Capturing the long-sought small-bandgap endohedral fullerene Sc3N@C82 with low kinetic stability.
Wei, Tao; Wang, Song; Liu, Fupin; Tan, Yuanzhi; Zhu, Xianjun; Xie, Suyuan; Yang, Shangfeng; Journal of the American Chemical Society 137 (2015) 3119–3123; doi:10.1021/jacs.5b00199

data_4129291
_publ_section_title
;
 Capturing the long-sought small-bandgap endohedral fullerene Sc3N@C82
 with low kinetic stability.
;
_journal_issue                   8
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3119
_journal_page_last               3123
_journal_paper_doi               10.1021/jacs.5b00199
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C130.75 H56 N5 Ni Sc3'
_chemical_formula_weight         1890.40
_chemical_name_common            ;Sc3N@C2v(39718)-C82/Ni(OEP)/2benzene;
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.772(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.2209(5)
_cell_length_b                   15.1985(3)
_cell_length_c                   19.9181(4)
_cell_measurement_reflns_used    2936
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      70.3100
_cell_measurement_theta_min      3.9710
_cell_volume                     7608.5(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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      100.01(10)
_diffrn_detector_area_resol_mean 10.3415
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25282
_diffrn_reflns_theta_full        70.79
_diffrn_reflns_theta_max         70.79
_diffrn_reflns_theta_min         3.52
_exptl_absorpt_coefficient_mu    3.045
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3866
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1034
_refine_ls_number_reflns         7517
_refine_ls_number_restraints     1075
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0721
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1352P)^2^+30.4637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1983
_refine_ls_wR_factor_ref         0.2034
_reflns_number_gt                6807
_reflns_number_total             7517
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b00199_si_002.cif
_cod_data_source_block           sc3n@c82
_cod_database_code               4129291