Preparation of Trimeric and Tetrameric Bis(trifluoromethyl)arsazene; X-Ray Study of 4

Article abstract of DOI:10.1039/DT9830001011

Two new aminoarsines, (CF3)2AsN(SiMe3)2 (1) and CF3As2 (2), are formed by reaction of (CF3)2AsCl and (CF3)AsCl2 with LiN(SiMe3)2.Chlorination of (1) yields <(CF3)2As(Cl)N(SiMe3)>2 (3).On refluxing (3) in n-hexane or n-heptane, the synthesis of trimeric and tetrameric bis(trifluoromethyl)arsazenes, <(CF3)2AsN>3 (4) and <(CF3)2AsN>4 (5), is accomplished.Pyrolysis of (3) also produced (4) and (5).Crystals of (5) are triclinic, space group P1, with a = 991.2(5), b = 1012.9(6), c = 1432.8(7) pm, α = 108.21(4), β = 96.03(4), γ = 109.44(4) deg, and Z = 2.The structure was solved by direct methods and refined to R 0.069 for 2183 unique observed diffractometer data.The molecular symmetry approximates to 4 (S₄), with a slight alternation in As-N distances <171.6(7) and 173.2(9) pm>.

Full text of DOI:10.1039/DT9830001011

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