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硫属元素二甲基镓酸盐和 - 铟酸盐DMPyr [Me M(μ -E)] （M = Ga，In；E = S，Se）：高阶和低阶硫属元素铟酸盐的结构单元

Chalcogenido-Dimethylgallates and -Indates DMPyr [Me M(μ -E)] (M=Ga, In; E=S, Se): Building Blocks for Higher and Lower Order Chalcogenidoindates.

作者信息

Guschlbauer Jannick, Vollgraff Tobias, Finger Lars H, Harms Klaus, Sundermeyer Jörg

机构信息

Fachbereich Chemie and Materials Science Center, Philipps-Universität, Hans-Meerwein-Str. 4, 35032, Marburg, Germany.

出版信息

ChemistryOpen. 2021 Feb;10(2):83-91. doi: 10.1002/open.202000347.

DOI:10.1002/open.202000347
PMID:33565735
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC7874246/
Abstract

Metalation of the anions in the ionic liquids DMPyr[SH] and DMPyr[SeH] (DMPyr=1,1-dimethylpyrrolidinium) by trimethylgallium and trimethylindium is investigated. The reaction proceeds via pre-coordination of [EH] , methane elimination and formation of an unprecedented series of chalcogenido metalates DMPyr [Me M(μ -E)] (M=Ga, In; E=S, Se). These show the presences of dinuclear dianions with four-membered ring structures displaying highly nucleophilic bridging chalcogenide ligands in their crystallographically determined molecular structures. Some representative reactions of these building blocks with amphoteric electrophiles were studied: Addition of two equivalents of E(SiMe ) (E=S, Se) to the indates DMPyr [Me In(μ -S)] and DMPyr [Me In(μ -Se)] leads to a cleavage of the ring, E silylation and formation of mononuclear, monoanionic indates DMPyr[Me In(SSiMe ) ], DMPyr[Me In(SeSiMe ) ], and even a mixed sulfido-selenido dimethylindate DMPyr[Me In(SSiMe )(SeSiMe )]. Reaction of DMPyr [Me In(μ -S)] with two equivalents of Lewis acid Me In leads to charge delocalization, ring expansion and formation of six-membered ring DMPyr [Me In(μ -S-InMe )] . The latter is a key intermediate in the formation of dianionic sulfidoindate DMPyr [(Me In) (μ -S) ] displaying an unusual inverse heteroadamantane cage structure with four capping sulfido ligands.

摘要

研究了三甲基镓和三甲基铟对离子液体DMPyr[SH]和DMPyr[SeH]（DMPyr = 1,1 - 二甲基吡咯烷鎓）中阴离子的金属化作用。该反应通过[EH]的预配位、甲烷消除以及形成一系列前所未有的硫属金属酸盐DMPyr [MeM(μ - E)]（M = Ga，In；E = S，Se）来进行。这些化合物在其晶体学确定的分子结构中显示出具有四元环结构的双核二价阴离子的存在，其中桥连硫属化物配体具有高亲核性。研究了这些结构单元与两性亲电试剂的一些代表性反应：向铟酸盐DMPyr [MeIn(μ - S)]和DMPyr [MeIn(μ - Se)]中加入两当量的E(SiMe₃)（E = S，Se）会导致环裂解、E硅烷化并形成单核单阴离子铟酸盐DMPyr[MeIn(SSiMe₃)]、DMPyr[MeIn(SeSiMe₃)]，甚至还有混合硫代 - 硒代二甲基铟酸盐DMPyr[MeIn(SSiMe₃)(SeSiMe₃)]。DMPyr [MeIn(μ - S)]与两当量的路易斯酸Me₂In反应会导致电荷离域、环扩张并形成六元环DMPyr [MeIn(μ - S - InMe₂)]。后者是形成二价阴离子硫代铟酸盐DMPyr [(Me₂In)₂(μ - S)₂]的关键中间体，该硫代铟酸盐具有不寻常的反式杂金刚烷笼状结构，带有四个封端硫代配体。

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