Detection of a Family of Gadolinium-Containing Endohedral Fullerenes and the Isolation and Crystallographic Characterization of One Member as a Metal-Carbide Encapsulated inside a Large Fullerene Cage
Hua Yang; Chunxin Lu; Ziyang Liu; Hongxiao Jin; Yuliang Che; Marilyn M. Olmstead; Alan L. Balch; Journal of the American Chemical Society 130 (2008) 17296–17300; doi:10.1021/ja8078303

data_4108902
_publ_section_title
;
 Detection of a Family of Gadolinium-Containing Endohedral Fullerenes and
 the Isolation and Crystallographic Characterization of One Member as a
 Metal-Carbide Encapsulated inside a Large Fullerene Cage
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17296
_journal_page_last               17300
_journal_paper_doi               10.1021/ja8078303
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'Gd2 C94, Ni N4 C38 H44, 2(C6 H6)'
_chemical_formula_sum            'C142 H56 Gd2 N4 Ni'
_chemical_formula_weight         2191.12
_chemical_name_common            Gd2(C2)@C92.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                 97.222(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.2381(14)
_cell_length_b                   17.6005(10)
_cell_length_c                   19.7867(12)
_cell_measurement_reflns_used    9131
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.7
_cell_volume                     8374.1(8)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'Apex2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART 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  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            48440
_diffrn_reflns_theta_full        28.19
_diffrn_reflns_theta_max         28.19
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    1.859
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             4368
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.679
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         10532
_refine_ls_number_restraints     360
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1589
_refine_ls_R_factor_gt           0.1150
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1875P)^2^+99.9126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3151
_refine_ls_wR_factor_ref         0.3576
_reflns_number_gt                6945
_reflns_number_total             10532
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja8078303_si_001.cif
_cod_data_source_block           mn1874
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4108902