Isolation and Structural Characterization of a Family of Endohedral Fullerenes Including the Large, Chiral Cage Fullerenes Tb3N@C88 and Tb3N@C86 as well as the Ih and D5h Isomers of Tb3N@C80
Tianming Zuo; Christine M. Beavers; James C. Duchamp; Anne Campbell; Harry C. Dorn; Marilyn M. Olmstead; Alan L. Balch; Journal of the American Chemical Society 129 (2007) 2035–2043; doi:10.1021/ja066437+

data_4111328
_publ_section_title
;
 Isolation and Structural Characterization of a Family of Endohedral
 Fullerenes Including the Large, Chiral Cage Fullerenes Tb3N@C88 and
 Tb3N@C86 as well as the Ih and D5h Isomers of Tb3N@C80
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2035
_journal_page_last               2043
_journal_paper_doi               10.1021/ja066437+
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C80 N Tb3, C36 H44 N4 Ni, 2(C6 H6)'
_chemical_formula_sum            'C128 H56 N5 Ni Tb3'
_chemical_formula_weight         2199.25
_chemical_name_common            Tb3N@C80(Ih).NiOEP.2benzene
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 95.2030(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.3036(8)
_cell_length_b                   15.0584(5)
_cell_length_c                   39.3947(13)
_cell_measurement_reflns_used    7648
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      2.5
_cell_volume                     14948.8(8)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0423
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            120596
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.68
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.124
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             8656
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.276
_refine_diff_density_min         -1.969
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1276
_refine_ls_number_reflns         22794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+42.3774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0825
_reflns_number_gt                17724
_reflns_number_total             22794
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja066437si20060906_013236.cif
_cod_data_source_block           mn1790
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4111328