Unique reactivity of a tetradentate N(2)S(2) complex of nickel: intermediates in the production of sulfur oxygenates

Inorganic Chemistry
Vincent E KaasjagerLisa M Thomson

Abstract

Complex 1 [(N,N'-dimethyl-N,N'-bis(2-sulfanylethyl)ethylenediamine)nickel(II)], previously shown to react with H(2)O(2) to produce the fully oxygenated disulfonate 5 [diaqua(N,N'-dimethyl-N,N'-bis(2-sulfonatoethyl)ethylenediamine)nickel(II)], has been explored in detail to explain the observed reactivity of this compound and to discern intermediates in the oxygenation reaction. Reaction of 1 with 1 equiv of methyl iodide results in the monomethylated square-planar nickel complex 2 [[(N,N'-dimethyl-N-(2-sulfanylethyl)-N'-(2-methylthioethyl)(ethylenediamine)nickel(II)] iodide], while a slight excess of methyl iodide results in the dimethylated complex 3 [diiodo(N,N'-dimethyl-N,N'-bis(2-methylthioethyl)ethylenediamine)nickel(II)], an X-ray structure of which has shown that the nickel ion is in an octahedral N(2)S(2)I(2) environment. Crystal data of 3: monoclinic, a = 8.865(3) A, b = 14.419(4) A, c = 14.389(6) A, beta = 100.19(3) degrees, V = 1810.2(12) A(3), space group P2(1)/n, Z = 4. The equatorial positions are occupied by the two cis-amine N-atoms and the coordinated iodides, while the axial positions are occupied by the thioether sulfur atoms. In organic solvents, the dithiolate complex 1 reacts with molecular oxygen or H(2)O...Continue Reading

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