M2@C79N (M = Y, Tb): Isolation and Characterization of Stable Endohedral Metallofullerenes Exhibiting M-M Bonding Interactions inside Aza[80]fullerene Cages
Tianming Zuo; Liaosa Xu; Christine M. Beavers; Marilyn M. Olmstead; Wujun Fu; T. Daniel Crawford; Alan L. Balch; Harry C. Dorn; Journal of the American Chemical Society 130 (2008) 12992–12997; doi:10.1021/ja802417d

data_4108388
_publ_section_title
;
 M2@C79N (M = Y, Tb): Isolation and Characterization of Stable Endohedral
 Metallofullerenes Exhibiting M-M Bonding Interactions inside
 Aza[80]fullerene Cages
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12992
_journal_page_last               12997
_journal_paper_doi               10.1021/ja802417d
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'Tb2 C80, C36 H44 N4 Ni, 2(C6 H6)'
_chemical_formula_sum            'C128 H56 N4 Ni Tb2'
_chemical_formula_weight         2026.32
_chemical_name_common            Tb2@C79N.NiOEP.2benzene
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 95.063(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.1848(7)
_cell_length_b                   15.1160(5)
_cell_length_c                   19.7406(7)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      34.0
_cell_measurement_theta_min      3.5
_cell_volume                     7485.8(4)
_computing_cell_refinement       'SAINT 7.16 (Bruker, 2005)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL 5.1 (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_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 Apex2'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source         'Advanced Light Source'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_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            101461
_diffrn_reflns_theta_full        31.57
_diffrn_reflns_theta_max         31.57
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    2.727
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/4 (Sheldrick, 2007)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_description       prism
_exptl_crystal_F_000             4040
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.264
_refine_diff_density_min         -1.930
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         10012
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0844
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1363P)^2^+55.8103P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2357
_refine_ls_wR_factor_ref         0.2435
_reflns_number_gt                8915
_reflns_number_total             10012
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja802417d_si_002.cif
_cod_data_source_block           mn1861
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4108388