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Separation And Characterization Of Isolated-Pentagon Rule Violating Chlorofullerenes (C64Cl4 And C56Cl10)

Posted on:2010-09-14Degree:MasterType:Thesis
Country:ChinaCandidate:X HanFull Text:PDF
GTID:2121360275489797Subject:Inorganic Chemistry
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Since 1985 when fullerenes were first discovered, IPR-satisfying (IPR: Isolated Pentagon Rule) fullerenes have been synthesized and widely applied in various fields. However, it is still a challenge for the synthesis, isolation and characterization of non-IPR fullerenes. In this contribution, we synthesized two non-IPR fullerenes, namely C64Cl4 and C56Cl10, via modified graphite arc-discharge process by adding a small amount of chlorine (such as Cl2 or CCl4) into the buffer gas. These non-IPR fullerenes were isolated from the crude soot using multi-step high performance liquid chromatography (HPLC). The structure of purified materials was identified in terms of sigle-crystal X-ray diffraction。The crude soot synthesized by graphite arc-discharge, was extracted with toluene, followed by separation via HPLC. We selected toluene as the mobile phase, because of the well solubility of chlorofullerene in toluene. The pyrenebutyric acid bonded silica column, Buckyprep-M column and Buckyprep column were adopted for isolation of these chlorofullerenes.The structure of C3v-#1911C64Cl4 has been established by single-crystal X-ray diffraction. C3v-#1911C64Cl4 has a set of triply-directly-fused pentagons, whose fused pentagon sites are passivated by chlorines. By comparing the pyramidalization angle of the pristine cages and the chlorinated #1911C64, we found the sever decrease of pyramidalization angle after chlorination. Meanwhile the n-n interaction of #1911C64Cl4 molecules is considerable, implying the potential applications in molecular electronics because of the easier electron transfer between neighbouring fullerenes in the crystal.Besides, we successfully isolated another new non-IPR fullerene #913C56Cl10 by HPLC. In order to purify this non-IPR fullerene, four steps of separation were adopted. The fundamental studies for non-IPR fullerenes separation would facilitate the further investigations on related fullerene materials.
Keywords/Search Tags:non-IPR Fullerenes, Seperation, #1911C64Cl4, #913C56Cl10
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