Synthesis and Characterisation of Ternary Cage Compounds with Adamantane‐Like M
<sub>4</sub>
P
<sub>4</sub>
Si
<sub>2</sub>
(M = Al, Ga, In) Core Structures
作者:Carsten von Hänisch
DOI:10.1002/ejic.200300156
日期:2003.8
isotypical in the triclinic space group P ; the lattice constants are: 3: a = 1129.0(6), b = 1164.8(8), c = 1750.6(8) pm; α = 83.63(5), β = 81.53(4), γ = 73.39(5)°; 4: a = 1125.9(7), b = 1159.0(7), c = 1744.7(7) pm; α = 83.71(4), β = 81.89(4), γ = 73.05(5)°; 5: a = 1147.4(2), b = 1174.7(2), c = 1753.3(4) pm; α = 85.32(3), β = 82.03(3), γ = 73.40(3)°. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim
[LiAl(PH2)4] 或 [NaAl(PH2)4] 与 Et2SiCl2 或 iPr2SiCl2 的反应分别产生二烷基二膦基硅烷 Et2Si(PH2)2 (1) 和 iPr2Si(PH2)2 (2)。两种化合物均通过核磁共振光谱法和质谱法进行鉴定。化合物 2 与 MEt3 (M = Al, Ga, In) 反应形成笼状化合物 [iPr2SiP(H)MEt2}2]2 (3: M = Al, 4: M = Ga, 5: M = In) . 这三个簇通过核磁共振和红外光谱以及单晶 X 射线衍射进行了充分表征。3-5 的中心结构基序是一个由四个金属、四个磷和两个硅原子组成的金刚烷笼。它们是第一个具有这些元素组合的三元团簇,并在三斜空间群 P 中同型结晶;晶格常数为: 3: a = 1129.0(6), b = 1164.8(8), c = 1750.6(8) pm; α = 83.63(5)