Abstract
The reaction of [Pd 4(μ-CO) 4(μ-O 2CCH 3) 4] with C 8H 9NC has been shown to occur with substitution of CO by C 8H 9 NC to give [Pd 4(μ-CO) 2(μ-CNC 8H 9) 2(μ-O 2CCH 3) 4] ( 1 with two equivalents of isocyanide and [Pd 4(μ-CNC 8H 9) 4(μ-O 2CCH 3) 4] ( 2) with four equivalents of isocyanide. The structure of [Pd 4(μ-CNC 8H 9) 4(μ-O 2CCH 3) 4]· CH 2Cl 2 has been determined by single crystal X-ray diffractometry. The structure is based on a rectangular unit of palladium atoms with the two shorter edges, which have PdPd distances of 2.6572(5) and 2.6668(4) åA, bridged by isocyanide ligands, and the two longer edges, with PdPd distances of 2.8888(4) and 2.9369(4) åA, bridged by two acetate ligands. The bridging isocyanide groups are nearly linear, with CNC angles of between 161.2(4) and 169.3(5)°. This leads to relatively high values for the v(NC) stretching frequencies in the IR spectrum. Compound 1 has also been synthesised by carbon monoxide reduction of palladium(II) acetate in the presence of isocyanide.
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