Tb3N@C84: an improbable, egg-shaped endohedral fullerene that violates the isolated pentagon rule.
Beavers, Christine M; Zuo, Tianming; Duchamp, James C; Harich, Kim; Dorn, Harry C; Olmstead, Marilyn M; Balch, Alan L; Journal of the American Chemical Society 128 (2006) 11352–11353; doi:10.1021/ja063636k

data_4101580
_publ_section_title
;
 Tb3N@C84: an improbable, egg-shaped endohedral fullerene that violates
 the isolated pentagon rule.
;
_journal_issue                   35
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11352
_journal_page_last               11353
_journal_paper_doi               10.1021/ja063636k
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C84 N Tb3, C36 H44 N4 Ni, 2(C6 H6)'
_chemical_formula_sum            'C132 H56 N5 Ni Tb3'
_chemical_formula_weight         2247.29
_chemical_name_common
;
(Tb~3~N@C~84~)(Ni(OEP) &#x00B7; 2 benzene
;
_chemical_name_systematic
; 
 (\m ~3~-Nitrido)-\h ^6^, \h^4^,\h^5^-C84 Fullerene)-triterbium (2,3,7,8,12,13,17,18-octaethylporphyrinato)nickel(II) benzene disolvate
;
_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                85.231(2)
_cell_angle_beta                 89.668(2)
_cell_angle_gamma                62.199(2)
_cell_formula_units_Z            2
_cell_length_a                   14.5782(13)
_cell_length_b                   15.0328(14)
_cell_length_c                   19.725(2)
_cell_measurement_reflns_used    7631
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25.9305
_cell_measurement_theta_min      2.4685
_cell_volume                     3807.9(6)
_computing_cell_refinement       'SAINT 7.16 (Bruker, 2005)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1698
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19031
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.77
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.068
_exptl_absorpt_correction_T_max  0.8567
_exptl_absorpt_correction_T_min  0.7697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.960
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       paralellipiped
_exptl_crystal_F_000             2212
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.139
_refine_diff_density_min         -1.410
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.814
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     968
_refine_ls_number_reflns         19037
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.814
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0976
_reflns_number_gt                10509
_reflns_number_total             19037
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja063636ksi20060706_070100.cif
_cod_data_source_block           twin
_cod_database_code               4101580