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Synthesis of heterometallic carbide clusters containing three iron atoms: (PPN)/sup 2/(MFe/sub 3/(CO)/sub 13/C) (M = Cr, W), (PPN)/sub 2/(Cr/sub 2/Fe/sub 3/(CO)/sub 16/C), Rh/sub 2/Fe/sub 3/(CO)/sub 14/C, and (PPN)(Rh/sub 3/Fenumber(CO)/sub 15/C)

Journal Article · · Inorg. Chem.; (United States)
DOI:https://doi.org/10.1021/ic00265a006· OSTI ID:6087334
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Redox-condensation reactions involving (PPN)/sub 2/(Fe/sub 3/(CO)/sub 9/(CCO)) and electrophilic transition-metal reagents lead to (PPN)/sub 2/(MFe/sub 3/(CO)/sub 13/C) (M = Cr, W), (PPN)/sub 2/(Cr/sub 2/Fe/sub 3/(CO)/sub 16/C), Rh/sub 2/Fe/sub 3/(CO)/sub 14/C, and (PPN)(Rh/sub 3/Fe/sub 3/(CO)/sub 15/C). Variable-temperature /sup 13/C NMR spectroscopy was employed to assign the structures of the tetranuclear clusters and Rh/sub 2/Fe/sup 3/(CO)/sub 14/C in solution. An improved synthesis of (PPN)(RhFe/sub 3/(CO)/sub 12/C) and more complete variable-temperature (ca. -130 to +20 /sup 0/C) /sup 13/C NMR spectra of this cluster and (PPN)(MnFe/sub 3/(CO)/sub 13/C) are discussed. All of the tetranuclear clusters are assigned butterfly metal geometries will the heterometals located at hinge sites. Attempts to prepare iron-molybdenum carbide clusters are discussed. The structure of (PPN)(Rh/sub 3/Fe/sub 3/(CO)/sub 15/C) was determined by a single-crystal x-ray diffraction study and was found to consist of a trigonal-antiprismatic metal array with the carbide ligand within the metal polyhedron. The iron atoms define one of the trigonal faces and the rhodium atoms define the other. Crystal data for (PPN)(Rh/sub 3/Fe/sub 3/(CO)/sub 15/C): monoclinic, space group P2/sub 1//n, a = 16.220 (6) A, b = 9.282 (3) A, c = 35.17 (3) A, ..beta.. = 94.84 (5)/sup 0/, Z = 4. 28 references, 5 figures, 6 tables.

Research Organization:
Northwestern Univ., Evanston, IL
DOE Contract Number:
AC02-83ER13104; FG02-86ER13640
OSTI ID:
6087334
Journal Information:
Inorg. Chem.; (United States), Journal Name: Inorg. Chem.; (United States) Vol. 26:18; ISSN INOCA
Country of Publication:
United States
Language:
English

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Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400201* -- Chemical & Physicochemical Properties
CARBIDES
CARBON 13
CARBON COMPOUNDS
CARBON ISOTOPES
CHROMIUM CARBIDES
CHROMIUM COMPOUNDS
CRYSTAL STRUCTURE
DATA
EVEN-ODD NUCLEI
EXPERIMENTAL DATA
INFORMATION
IRON CARBIDES
IRON COMPOUNDS
ISOTOPES
LIGHT NUCLEI
NITROGEN COMPOUNDS
NMR SPECTRA
NUCLEI
NUMERICAL DATA
PHOSPHORUS COMPOUNDS
REFRACTORY METAL COMPOUNDS
RHODIUM COMPOUNDS
SPECTRA
STABLE ISOTOPES
SYNTHESIS
TRANSITION ELEMENT COMPOUNDS
TUNGSTEN CARBIDES
TUNGSTEN COMPOUNDS