Is the Isolated Pentagon Rule Merely a Suggestion for Endohedral Fullerenes? The Structure of a Second Egg-Shaped Endohedral Fullerene-Gd3N@Cs(39663)-C82
Brandon Q. Mercado; Christine M. Beavers; Marilyn M. Olmstead; Manuel N. Chaur; Kenneth Walker; Brian C. Holloway; Luis Echegoyen; Alan L. Balch; Journal of the American Chemical Society 130 (2008) 7854–7855; doi:10.1021/ja8032263

data_4107932
_publ_section_title
;
 Is the Isolated Pentagon Rule Merely a Suggestion for Endohedral
 Fullerenes? The Structure of a Second Egg-Shaped Endohedral
 Fullerene-Gd3N@Cs(39663)-C82
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7854
_journal_page_last               7855
_journal_paper_doi               10.1021/ja8032263
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C130 H56 Gd3 N5 Ni'
_chemical_formula_weight         2218.26
_chemical_name_common            'Gd3N@C82.NiOEP.2benzene nonIPR isomer 39663'
_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                85.636(2)
_cell_angle_beta                 88.659(2)
_cell_angle_gamma                61.500(1)
_cell_formula_units_Z            2
_cell_length_a                   14.6044(17)
_cell_length_b                   14.9475(17)
_cell_length_c                   19.842(2)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.7
_cell_measurement_theta_min      2.7
_cell_volume                     3795.1(7)
_computing_cell_refinement       'SAINT 7.16 (Bruker, 2007)'
_computing_data_collection       'Apex2 (Bruker, 2007)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART ApexII'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  silicon(111)
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22989
_diffrn_reflns_theta_full        31.65
_diffrn_reflns_theta_max         31.65
_diffrn_reflns_theta_min         2.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.632
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS v2007/3 (Sheldrick, 2007)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.941
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2182
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.546
_refine_diff_density_min         -1.784
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1401
_refine_ls_number_reflns         19622
_refine_ls_number_restraints     123
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0804P)^2^+8.4132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.1792
_reflns_number_gt                13285
_reflns_number_total             19622
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja8032263-file001.cif
_cod_data_source_block           cb84
_cod_original_cell_volume        3795.2(7)
_cod_database_code               4107932