화학공학소재연구정보센터
Inorganic Chemistry, Vol.38, No.12, 2957-2960, 1999
Reactions of LiE(SiMe3)(3), E = Si, Ge: X-ray crystal structure of the cyclotetrastannane [ClSnSi(SiMe3)(3)](4)
Reaction of SnCl2. dioxane with 2 equiv of Li(THF)(3)Si(SiMe3)(3) in hexane afforded the cyclotetrastannane [(Me3Si)(3)SiSnCl](4) in reasonable yield. From pentane, the product crystallized as a red-orange disolvate in the P (1) over bar space group (triclinic) with a = 14.735(2) Angstrom, b = 14.976(2) Angstrom, c = 24.066(3) Angstrom, alpha = 76.94 degrees, beta = 76.19 degrees, gamma = 62.11 degrees, V = 4517.5 Angstrom(3), and Z = 2. The Sn-4 ring consisted of a slightly distorted, nonplanar (fold angle = 18.9 degrees) rectangle with Sn-Sn distances of 2.8054(6), 2.8111(6), 2.9122(6), and 2.9146(6) Angstrom. The pentane molecules were disordered. Selected mono- and dihalogermanes were treated with 1 equiv of Li(THF)3Si(SiMe3)3 or Li(THF)(2.5)Ge(SiMe3)(3), affording (Me3Si)(3)EGe(CF3)(3) (E = Si, Ge) and (Me3Si)(3)GeGeR3 (R = Cl, CH3, C6H5). Besides the monosubstitution product, the reaction of GeCl4 with 1 equiv of Li(THF)(2.5)Ge(SiMe3)3 also gave a small amount of the linear tetragermane (Me3Si)(3)GeGeCl2GeCl2Ge(SiMe3)(3). Good yields of the analogous phenyl derivative, (Me3Si)(3)GeGePh2GePh2Ge(SiMe3)(3), were obtained by treating Ph2GeCl2 with 2 equiv of the lithium-germyl reagent.