The reactions of trimethylaluminum with diphenylarsine, Ph 2 AsH, and phenyl [(trimethylsilyl)methyl]arsine, Ph(Me 3 SiCH 2 )AsH, in 1:1 mole ratios afford the trimeric compounds [Me 2 AlAsPh 2 ] 3 ‚(C 7 H 8 ) 2 (1) and [Me 2 AlAs(CH 2 SiMe 3 )Ph] 3 (2), respectively. Compounds 1 and 2 are the first Al-As six-membered-ring compounds to be structurally characterized by singlecrystal X-ray crystallography, as well as by 1 H and 13 C solution NMR spectroscopy. X-ray crystallographic analysis revealed that trimer 1 is a toluate that crystallizes in the monoclinic space group P2 1 /n, with a ) 14.549(6) Å, b ) 22.838(7) Å, c ) 16.891(4) Å, and β ) 105.12(5)°f or Z ) 4. Trimer 2 crystallizes in the triclinic system, space group P1 h, and has two unique molecules in a unit cell with dimensions of a ) 15.619(7) Å, b ) 17.487(6) Å, c ) 19.863(6) Å, R ) 94.86(3)°, β ) 101.41(3)°, and γ ) 113.34(3)°for Z ) 4. The six-membered Al-As rings in both 1 and 2 occupy chair conformations, furnishing both trimers with structural characteristics similar to those of cyclohexane. The Al and As centers of both 1 and 2 reside in pseudotetrahedral environments, with the Al-As bond lengths ranging from 2.512(3) to 2.542(3) Å in 1 and from 2.504(5) to 2.526(5) Å in 2.
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