Partial separation and structural characterization of C[sub 84] isomers by crystallization of ([eta][sup 2]-C[sub 84])Ir(CO)Cl(P(C[sub 6]H[sub 5])[sub 3])[sub 2]

Journal Article · Wed Mar 09 04:00:00 EST 1994 · Journal of the American Chemical Society; (United States)

DOI:https://doi.org/10.1021/ja00084a106· OSTI ID:7267399

Balch, A L; Ginwalla, A S; Lee, J W; Noll, B C; Olmstead, M M ^[1]

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1. Univ. of California, Davis, CA (United States)

Here we describe the results of reacting Ir(CO)Cl(PPh[sub 3])[sub 2] with C[sub 84]. In this case, not only is there the question of regioselectivity of addition, which was also a factor in the Ir(CO)Cl(PPh[sub 3])[sub 2]/C[sub 70] reaction, but there is also the question of selectivity between the isomeric forms of C[sub 84] itself. C[sub 84] was prepared by the contact arc process and separated from other fullerenes by high-pressure liquid chromatography. Treatment of a saturated benzene solution of a triply chromatographed sample of C[sub 84] with a 21-fold molar excess of Ir(CO)Cl(PPh[sub 3])[sub 2] produced a green-brown solution, from which black crystals of ([eta][sup 2]-C[sub 84])Ir(CO)Cl(PPh[sub 3])[sub 2][center dot]4C[sub 6]H[sub 6] were obtained by slow diffusion of diethyl ether into the mixture. The structure of the complex as determined by a single-crystal X-ray diffraction study is shown. While the complex itself has no crystallographically imposed symmetry, the geometry of the C[sub 84] moiety does correspond to that of the D[sub 2d] (23) isomer. The distance along the principal axis that bisects the C(32)-C(53) and C(42)-C(43) bonds is 9.61 [angstrom], while the distance across the two axes that are perpendicular to this is 8.34 [angstrom]. Within D[sub 2d] symmetry, there are 19 different sets of C-C bonds for C[sub 84]. 18 refs.

• OSTI ID: 7267399
• Journal Information: Journal of the American Chemical Society; (United States), Journal Name: Journal of the American Chemical Society; (United States) Vol. 116:5; ISSN JACSAT; ISSN 0002-7863
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400105 -- Separation Procedures
400201* -- Chemical & Physicochemical Properties
CARBON
CHEMICAL BONDS
CHLORINE COMPOUNDS
CHROMATOGRAPHY
COHERENT SCATTERING
COMPLEXES
CRYSTALLIZATION
DIFFRACTION
ELEMENTS
FULLERENES
HALOGEN COMPOUNDS
IRIDIUM COMPLEXES
ISOMERS
NONMETALS
ORGANIC COMPOUNDS
ORGANOMETALLIC COMPOUNDS
PHASE TRANSFORMATIONS
SCATTERING
SEPARATION PROCESSES
TRANSITION ELEMENT COMPLEXES
X-RAY DIFFRACTION