Fachbereich Chemie and Wissenschaftliches Zentrum für Materialwissenschaften (WZMW), Philipps-Universität Marburg, Hans-Meerwein-Straße 4, 35043, Marburg, Germany.
Angew Chem Int Ed Engl. 2022 Dec 23;61(52):e202213098. doi: 10.1002/anie.202213098. Epub 2022 Nov 28.
Alkali metal dihydrogen-antimonides [M(L) SbH ], short: alkali metal antimonides (M=Li, Na, K, Rb, Cs; 1: L=pmdta; 2: L=crown-ether), were prepared from stibine and n-Butyllithium, M(hmds) (hmds=hexamethyldisilazane) or MOtBu, respectively. We developed a generally applicable synthesis route for these compounds and the obtained compounds were examined on their stability depending on the alkali metal and stabilizing additives used, whereby the use of appropriate crown-ethers allowed their isolation and characterization at room temperature. Moreover, the 1,4-dioxane adduct [Na(dioxane) SbH ] was the appropriate starting compound for the synthesis of the first primary silylstibane (Me Si) SiSbH (3) which was characterized by NMR and IR spectroscopy. Reaction of 3 with (Dipp NacNac)Ga (Dipp NacNac=HC{C(Me)N(Dipp)} ; Dipp=2,6-iPr C H ) resulted in the formation of (Dipp NacNac)GaH(SbHSi(SiMe ) ) (4) which was furthermore characterized by single crystal x-ray diffraction.
碱金属二氢锑化物[M(L)SbH ]，简称碱金属锑化物（M=Li、Na、K、Rb、Cs；1：L=pmdta；2：L=冠醚），由胂和正丁基锂、M（hmds）（hmds=六甲基二硅氮烷）或 MOtBu 分别制备而成。我们开发了一种适用于这些化合物的通用合成路线，并根据所用的碱金属和稳定添加剂考察了它们的稳定性，其中适当的冠醚的使用允许在室温下对其进行分离和表征。此外，1,4-二氧杂环己烷加合物[Na(dioxane)SbH ]是合成第一个仲硅基锑烷（Me Si）SiSbH（3）的合适起始化合物，该化合物通过 NMR 和 IR 光谱进行了表征。3 与（Dipp NacNac）Ga（Dipp NacNac=HC{C(Me)N(Dipp)}；Dipp=2,6-iPr C H ）反应生成（Dipp NacNac）GaH(SbHSi(SiMe ) )（4），该化合物还通过单晶 X 射线衍射进行了表征。
