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Article type: Research Article
Authors: Cowley, Alan H. | Gabbaï, François P. | Isom, Harold S. | Decken, Andreas | Culp, Robert D.
Affiliations: Department of Chemistry and Biochemistry, The University of Texas at Austin, Austin, Texas 78712
Abstract: The reactions of the “two-arm” arylithium [2, 6-(Me2NCH2)2C6H3]Li with InI3, and i-PrInI2 afforded the diiodide [2, 6-(Me2NCH2)2C6H3]InI2(3) and the monoiodide [{2,6-(Me2NCH2)2C6H3){i-Pr}InI]∞ (4), respectively. The corresponding “one-arm” derivatives [{2-(Me2NCH2)C6H4}InI2]2 (5) and [{2-(Me2NCH2)C6H4}{i-Pr}InI]2 (6) were formed via the reactions of [2-(Me2NCH2)C6H4]Li with InI3 and i-PrInI2, respectively. The four new compounds have been characterized on the basis of elemental analysis, 1H and 13C NMR, and mass spectroscopy. The solid-state structures of (3-6) have been established by X-ray crystallography: (3), is monomeric, (5), and (6) are dimeric, and (4) possesses a zig-zag chain-type structure with In-I-In bridges. Single-crystal data are as follows: (3), triclinic, P1, with a = 8.951(1)Å, b = 11.523(1)Å c = 16.988(1)Å, α = 87.05(1)°, β = 88.51(1)°, γ = 84.73(1)°, V = 1742.1(3)Å3, Z = 4, d (calcd) = 2.135 gcm−3, 5670 observed reflections, and R = 0.0465 (Rw = 0.0558); (4), monoclinic, Cc, with a = 9.055(1)Å, b = 25.683(4)Å, c = 15.865(3)Å, β = 90.49(l)°, V = 3690(2)Å3, Z = 8, d (calcd) = 1.714 gcm−3, 3895 observcd reflections, and R = 0.0761 (Rw = 0.1038); (5), triclinic, P1, with a = 8.783(1)Å, b = 8.976(1)Å, c = 18.493(3)Å, α = 99.42(1)°, β = 93.64(1)°, γ = 110.31(1)°, V = 1337.4(3)Å3, Z = 4, d (calcd) = 2.497 g cm−3, 5427 observed reflections, and R = 0.0560 (Rw = 0.1212); (6), monoclinic, P21/n, with a = 9.637(2)Å, b = 16.162(2)Å, c = 10.317(1)Å β = 114.04(2)°, V = 1467.6(7)Å3, Z = 4, d (calcd) = 1.896 g cm−3, 2578 observed reflections, and R = 0.0474 (Rw = 0.0419).
DOI: 10.1080/13583149512331338225
Journal: Main Group Chemistry, vol. 1, no. 1, pp. 9-19, 1995
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