Selective Synthesis, Isolation, and Crystallographic Characterization of LaSc2N@I-h-C-80
Chemistry and Biochemistry
The successful preparation and isolation of the mixed-metal endohedral fullerene, LaSc2N@I-h-C-80, and its structural characterization by single-crystal X-ray diffraction are reported. Results from chemically adjusting plasma temperature, energy, and reactivity (CAPTEAR) experiments indicate that a 10 wt % addition of Cu(NO3)(2)center dot 2.5H(2)O to a mixture of La2O3 and Sc2O3 decreases the amount of C-60 and C-70 found in soot extracts by an order of magnitude. By combining a stoichiometric 2-fold excess of La to Sc atoms in the plasma reactor, an extract containing a greater abundance of LaSc2N@I-h-C-80 relative to Sc3N@I-h-C-80 was obtained. Alternatively, the stir and filter approach (SAFA method) can be used to remove the empty cage fullerenes from a carbon soot sample prepared without using Cu(NO3)(2)center dot 2.5H(2)O. LaSc2N@I-h-C-80 has been characterized by UV/vis absorption spectroscopy and by single-crystal X-ray diffraction. Ordered crystals with nearly identical orientations of the endohedral relative to the porphyrin have been obtained by cocrystallization of LaSc2N@I-h-C-80 with either Ni-II(OEP) or H-2(OEP). The LaSc2N unit is planar, although earlier computations suggested that it would be pyramidal.
Rose, C. B.,
Maslenikova, J. S.,
Villarreal, J. R.,
Mackey, M. A.,
Mercado, B. Q.,
Olmstead, M. M.,
Balch, A. L.
(2012). Selective Synthesis, Isolation, and Crystallographic Characterization of LaSc2N@I-h-C-80. Inorganic Chemistry, 51(24), 13096-81.
Available at: http://aquila.usm.edu/fac_pubs/7561