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_4111329
_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_sum            'C139 H59 N5 Ni Tb3'
_chemical_formula_weight         2334.38
_chemical_name_common            Tb3N@(D2-35)C88.NiOEP.2.5benzene
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.940(3)
_cell_angle_beta                 76.268(3)
_cell_angle_gamma                65.161(3)
_cell_formula_units_Z            2
_cell_length_a                   14.990(3)
_cell_length_b                   16.795(3)
_cell_length_c                   18.408(3)
_cell_measurement_reflns_used    6296
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.9
_cell_measurement_theta_min      2.4
_cell_volume                     4053.9(13)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'Apex2 (Bruker, 2006)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (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 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker ApexII'
_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  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            52427
_diffrn_reflns_theta_full        31.58
_diffrn_reflns_theta_max         31.58
_diffrn_reflns_theta_min         1.74
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.886
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2004)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2302
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.665
_refine_diff_density_min         -1.519
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.836
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1319
_refine_ls_number_reflns         30087
_refine_ls_number_restraints     908
_refine_ls_restrained_S_all      0.840
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.054
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1209
_reflns_number_gt                14648
_reflns_number_total             30087
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja066437si20060906_013259.cif
_cod_data_source_block           mn1799
_cod_database_code               4111329