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Copper(I)−acetonitrile complexes are exceedingly useful starting materials for the synthesis of copper(I) complexes with polydentate ligands. To extend the utility of such chemistry to solution studies in relatively low-dielectric solvents (i.e., diethyl ether, toluene) and to aid in obtaining products amenable to X-ray diffraction studies, we have recently begun to employ counteranions such as B(C₆F₅)₄^- for bioinorganic studies. Thus, the synthesis of [Cu(MeCN)₄]B(C₆F₅)₄ (1) is presented. Its recrystallization from CH₂Cl₂/pentane yields the linear, two-coordinate complex [Cu(MeCN)₂]B(C₆F₅)₄ (2), whose centrosymmetric X-ray structure shows that its Cu−N distance is significantly shorter than that in other two-coordinate Cu(I) complexes with nitrogen ligands or that in the tetrahedral complex [Cu(MeCN)₄]ClO₄. Infrared spectroscopy indicates interesting and diagnostically useful differences between the ν(CN) of 1 and 2.