Synthesis of a new endohedral fullerene family, Sc 2 2n (n = 40-50) by the introduction of SO 2
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1 Synthesis of a new endohedral fullerene family, Sc 2 S@C 2n (n = 40-50) by the introduction of SO 2 Ning Chen a, Manuel N. Chaur a,cheryl Moore a, Julio R. Pinzón a, Ramon Valencia b, Antonio Rodríguez-Fortea b, Josep M. Poblet *b and Luis Echegoyen *a a Department of Chemistry, Clemson University 219 Hunter Laboratories, Clemson, SC (USA). Fax: (+1) , luis@clemson.edu b Department de Química Fisica i Inorgànica, Universitat Rovira y Virgili c/ Marcel lí Domingo s/n, Campus Sescelades, E Tarragona (Spain), Fax: (+34) , josepmaria.poblet@urv.cat Experimental Details A mixture of scandium oxide and graphite powder was pressed into the hole of graphite-rods (POCO Co.) with a 1:3 weight ratio of scandium oxide and graphite powder. The packed rods were subjected to annealing at 1000 for 12 h. Fullerene soot is produced by arc-burning Sc 2 O 3 /graphite composite rods under an atmosphere of He (200 Torr)/ SO 2 (20 Torr) mixture. The generated soot was pre-extracted with acetone and further Soxlet-extracted with toluene for 12 h. The isolation of the Sc 2 S@C 82 from the asprepared fullerene mixture was accomplished by a multistep HPLC (Varian Pro Star 210) on Buckyprep-M (semi preparative, mm) and Buckyprep (semi preparative, mm) column. Mass spectra were measured by MALDI-TOF mass spectrometric analysis running in positive ion mode (Biflex Omni Flex, Germany). For the EDS analysis, the fullerene sample was first dispersed in an alcohol solution by ultrasonication and then deposited on a TEM grid. The spectrum was recorded on the HD-2000 STEM equipped with an Oxford EDS system. The UV-Vis- NIR spectrum was recorded on a Perkin LAMBDA 1050 UV/Vis/NIR spectrophotometer. Cyclic voltammetry experiments were performed on a BAS 100B workstation at room temperature under the protection of Argon gas flow. A 1-mm-diameter glassy carbon was used as the working electrode and a platinum wire and silver wire were employed as counter electrodes and reference electrode respectively. The supporting electrolyte, tetrabutylammonium- hexafluorophosphate, nbu 4 PF 6, electro chemical grade, Sigma Aldrich), was dried under reduced pressure at 340 K for 24 h and stored in a glove box prior to use. The concentration of nbu 4 PF 6 in o-dcb solutions was 0.05 mol/l. Ferrocene (Fc) was added as the internal standard for final voltammetric cycle and all potentials are referred to Fc/Fc + couple.
2 Figure S1. HPLC chromatogram of as-prepared scandium sulfide fullerene extract (obtained on a Buckyprep column with λ = 320 nm, a flow rate of 4 ml/min, and toluene as the eluent at 25 )
3 Figure S2. MALDI-TOF spectrum of the fullerene mixture from HPLC fraction 1.
4 Figure S3. MALDI-TOF spectrum of the fullerene mixture from HPLC fraction 2.
5 Figure S4. EDS spectrum of Sc 2 S@C 82 (I). Figure S5. EDS spectrum of Sc 2 S@C 82 (II)
6 Table S1 Relative stability ( E), ionization potential (IP), electron affinity (EA), electrochemical (EC) and HOMO-LUMO (H-L) gap computed for the two isomers of Sc 2 S@C 82. E a) IP b) EA b) EC b,c) H-L q d) Isomer I (C s :6) (1.46) Isomer II (C 3v :8) (1.56) a) Energy in kcal mol -1 ; b) Values computed in o-dcb are in ev and V for energies and potentials; c) Values in parenthesis correspond to the observed EC gap; d) Charge transfer computed for the internal cluster using AIM method. The atomic charge for Sc atoms is in average e. XYZ coordinates of computed structures For isomers I and II, ten and fourteen orientations of Sc 2 S inside the fullerene have been explored. Here we show the coordinates of those structures with the lowest energies (relative energies less than 4.5 kcal mol 1 ). Isomer I Sc 2 S@C s (6)-C 82 Orientation 3 E= ev C C C C C C C C C C C C C C C
7 C Sc C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C
8 C C C C C C C C C C C C C C C C C Sc C C C C C S Orientation 4 E= ev C C C C C C C C C C C C C C C C Sc C C
9 C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C
10 C C C C C C C C C C C C C Sc C C C C C S Orientation 5 E= ev C C C C C C C C C C C C C C C C Sc C C C C C C
11 C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C
12 C C C C C C C C C Sc C C C C C S Orientation 6 E= ev C C C C C C C C C C C C C C C C Sc C C C C C C C C C C
13 C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C
14 C C C C C Sc C C C C C S Isomer II Sc 2 S@C 3v (8)-C 82 Orientation 3 E= ev C C C C C C C C C C C C C C C C C C C C C C C C C C C C C
15 C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C
16 C C C C C C C S Sc Sc Orientation 4 E= ev C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C
17 C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C
18 C C C S Sc Sc Orientation 7 E= ev C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C
19 C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C S
20 Sc Sc Orientation 8 E= ev C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C
21 C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C S Sc Sc Orientation 10
22 E= ev C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C
23 C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C S Sc Sc Orientation 14 E= ev C C C
24 C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C
25 C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C C S Sc Sc
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