Large Metal Ions in a Relatively Small Fullerene Cage: The Structure of Gd3N@C2(22010)-C78 Departs from the Isolated Pentagon Rule
Christine M. Beavers; Manuel N. Chaur; Marilyn M. Olmstead; Luis Echegoyen; Alan L. Balch; Journal of the American Chemical Society 131 (2009) 11519–11524; doi:10.1021/ja903741r

data_4104871
_publ_section_title
;
 Large Metal Ions in a Relatively Small Fullerene Cage: The Structure of
 Gd3N@C2(22010)-C78 Departs from the Isolated Pentagon Rule
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11519
_journal_page_last               11524
_journal_paper_doi               10.1021/ja903741r
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C78 Gd3 N, C36 H44 N4 Ni, 1.5(C6 H6)'
_chemical_formula_sum            'C123 H53 Gd3 N5 Ni'
_chemical_formula_weight         2131.16
_chemical_name_common            Gd3N@C8.NiOEP.1.5benzene
_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                 94.2080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.9897(6)
_cell_length_b                   15.0876(4)
_cell_length_c                   39.2517(10)
_cell_measurement_reflns_used    9924
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      50.7
_cell_measurement_theta_min      2.4
_cell_volume                     14759.4(6)
_computing_cell_refinement       'SAINT v7.56A (Bruker, 2008)'
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  silicon(111)
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       78
_diffrn_reflns_limit_l_min       -78
_diffrn_reflns_number            567829
_diffrn_reflns_theta_full        51.54
_diffrn_reflns_theta_max         51.54
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    3.731
_exptl_absorpt_correction_T_max  0.7421
_exptl_absorpt_correction_T_min  0.6844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/1 (Shedrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.918
_exptl_crystal_description       block
_exptl_crystal_F_000             8368
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.085
_refine_diff_density_max         4.874
_refine_diff_density_min         -2.795
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2323
_refine_ls_number_reflns         63384
_refine_ls_number_restraints     5384
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1203
_refine_ls_R_factor_gt           0.0960
_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^)+(0.1591P)^2^+70.8248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2762
_refine_ls_wR_factor_ref         0.3026
_reflns_number_gt                47323
_reflns_number_total             63384
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja903741r_si_001.cif
_cod_data_source_block           cb118x
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4104871