Electrocrystallizing C[sub 60]. Synthesis, single crystal X-ray structure, and magnetic (ESR, SQUID) characterization of [(C[sub 6]H[sub 5])[sub 4]P][sub 2][C[sub 60]][1][sub x]

We report here on the synthesis by electrocrystallization of high quality single crystals of volume up to 1 mm[sup 3] of a salt of formula [(C[sub 6]H[sub 5])[sub 4]P][sub 2][C[sub 60]][I][sub x] (0 < x [much lt] 1), the description of its crystal and molecular structure, and its characterization...

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Bibliographic Details
Published in:Journal of the American Chemical Society 1993-11, Vol.115:22
Main Authors: Penicaud, A., Perez-Benitez, A., Gleason, V., Munoz P.E., Escudero, R.
Format: Article
Language:English
Subjects:
400102 - Chemical & Spectral Procedures
400201 - Chemical & Physicochemical Properties
CARBON
COHERENT SCATTERING
CRYSTALLIZATION
DIFFRACTION
ELECTRON SPIN RESONANCE
ELEMENTS
FULLERENES
INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY
MAGNETIC PROPERTIES
MAGNETIC RESONANCE
MOLECULAR STRUCTURE
NONMETALS
PHASE TRANSFORMATIONS
PHYSICAL PROPERTIES
RESONANCE
SCATTERING
SYNTHESIS
X-RAY DIFFRACTION
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Summary:We report here on the synthesis by electrocrystallization of high quality single crystals of volume up to 1 mm[sup 3] of a salt of formula [(C[sub 6]H[sub 5])[sub 4]P][sub 2][C[sub 60]][I][sub x] (0 < x [much lt] 1), the description of its crystal and molecular structure, and its characterization by NIR, EPR, and SQUID magnetic measurements. We have shown that the electrocrystallization technique can be successfully employed to grow large, high-quality single crystals of C[sub 60] salts suitable for X-rays as well as physical studies. The crystal structure of [(C[sub 6]H[sub 5])[sub 4]P][sub 2][C[sub 60]][I][sub x] shows fully isolated C[sub 60][sup [minus]] anions in a very symmetrical environment. 17 refs., 3 figs.
ISSN:0002-7863
1520-5126
DOI:10.1021/ja00075a078