Preparation of [K][In{Fe2(CO)8}2](THF) and Fe2{µ-InCl(THF)}2(CO)8 (THF = Tetrahydrofuran)

Chu Chieh Lin, Gapgoung Kong, Hyunho Cho, Bruce R. Whittlesey

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Abstract

The compound [K][In{Fe2(CO)8}2](THF) (1) (THF = tetrahydrofuran) has been synthesized by the reaction of Fe3(CO)12 with activated indium powder in the presence of potassium chloride. A single-crystal X-ray structure determination shows the iron atoms of two Fe2(CO)8 units bound to the indium in a pseudotetrahedral fashion and the potassium ion coordinated to a molecule of THF and two carbonyl oxygen atoms from each of four of the iron-indium anions to give a total coordination number of 9. Crystal data: tetragonal space group P4/n (No. 85), a = 11.850(2) Å, c = 10.696(2) Å, V = 1502.0(5) Å3, Z = 2, R = 3.61%, Rw = 5.04%. The complex Fe2{µ-InCl(THF)}2(CO)8 (2) can be prepared in high yield by the reaction of either Na2Fe(CO)4 or Na2Fe2(CO)8 with indium(III) chloride or via the reaction of Fe3(CO)12 with indium(I) chloride in tetrahydrofuran. Mechanistic studies suggest that these three reactions produce the same intermediate species, Fe(CO)4(THF) and InCl, which then combine to give the observed product. Fe2{µ-InCl(THF)}2(CO)8 forms an adduct with bromide ion in the presence of tetrabutylammonium bromide, and the complex [(C4H9)4N]2[Fe2{µ-InClBr}2(CO)8] (3) has been characterized crystallographically. Crystal data: triclinic space group P1̅ (No. 2), a = 11.510(2) Å, b = 11.905(1) Å, c = 12.200(2) Å, α = 90.373(9)°, β = 117.08(1)°, γ = 107.75(1)°, V = 1396.6(5) Å3, Z = 1, R = 4.61%, Rw = 5.94%.

Original languageEnglish
Pages (from-to)2705-2710
Number of pages6
JournalInorganic Chemistry
Volume32
Issue number12
DOIs
StatePublished - 1993

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