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Ionic Liquid‐Driven Formation of and Cation Exchange in Layered Sulfido Stannates – a CH2 Group Makes the Difference
ChemistryOpen ( IF 2.5 ) Pub Date : 2020-11-19 , DOI: 10.1002/open.202000287 Bertram Peters 1 , Martin Möbs 1 , Nick Michel 1 , Frank Tambornino 1 , Stefanie Dehnen 1
ChemistryOpen ( IF 2.5 ) Pub Date : 2020-11-19 , DOI: 10.1002/open.202000287 Bertram Peters 1 , Martin Möbs 1 , Nick Michel 1 , Frank Tambornino 1 , Stefanie Dehnen 1
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Two types of layered sulfido stannates or a molecular cluster compound are obtained upon ionothermal treatment of the simple sulfido stannate salt K4[SnS4] 
4H2O that is based on binary tetrahedral [SnS4]4− anions. The formation of the respective products, novel compounds (C4C1C1Im)2[Sn3S7] (1 a), (C4C1C2Im)2[Sn3S7] (1 b), and (C4C1C2Im)2[Sn4S9] (2) with layered anionic substructures, or the recently reported compound (C4C1C1Im)4+x[Sn10O4S16(SMe)4][An]x (A) comprising a molecular cluster anion, is controlled by both the choice of the ionic liquid cation and the reaction temperature. We report the scale‐up of the syntheses by a factor of 100 with regard to other reported ionothermal syntheses of related compounds, and a procedure of how to isolate them in phase‐pure form – both being rare observations in chalcogenido stannate chemistry in ionic liquids. Moreover, the synthesis of compound 1 a can be achieved by rapid cation exchange starting out from 1 b, which has not been reported for organic cations in any chalcogenido stannate salt to date.
中文翻译：
离子液体驱动的层状硫化锡酸盐的形成和阳离子交换——CH2 基团发挥作用
对简单的硫化锡酸盐K 4 [SnS 4 ]进行离子热处理，得到两种层状硫化锡酸盐或分子簇化合物。 4H 2 O 基于二元四面体 [SnS 4 ] 4−阴离子。各产物的形成，新化合物(C 4 C 1 C 1 Im) 2 [Sn 3 S 7 ] ( 1 a )、(C 4 C 1 C 2 Im) 2 [Sn 3 S 7 ] ( 1 b ) ，和(C 4 C 1 C 2 Im) 2 [Sn 4 S 9 ] ( 2 )，具有层状阴离子结构，或最近报道的化合物(C 4 C 1 C 1 Im) 4+x [Sn 10 O 4 S 16 (SMe) 4 ][An] x ( A )包含分子簇阴离子，通过离子液体阳离子的选择和反应温度两者来控制。我们报告了与其他报道的相关化合物的离子热合成相比，合成放大了 100 倍，以及如何以纯相形式分离它们的程序——这两者都是离子液体中硫族锡酸盐化学中罕见的观察结果。此外，化合物1a的合成可以通过从1b开始的快速阳离子交换来实现，迄今为止尚未报道任何硫族锡酸盐中的有机阳离子。
更新日期：2020-11-19
4H2O that is based on binary tetrahedral [SnS4]4− anions. The formation of the respective products, novel compounds (C4C1C1Im)2[Sn3S7] (1 a), (C4C1C2Im)2[Sn3S7] (1 b), and (C4C1C2Im)2[Sn4S9] (2) with layered anionic substructures, or the recently reported compound (C4C1C1Im)4+x[Sn10O4S16(SMe)4][An]x (A) comprising a molecular cluster anion, is controlled by both the choice of the ionic liquid cation and the reaction temperature. We report the scale‐up of the syntheses by a factor of 100 with regard to other reported ionothermal syntheses of related compounds, and a procedure of how to isolate them in phase‐pure form – both being rare observations in chalcogenido stannate chemistry in ionic liquids. Moreover, the synthesis of compound 1 a can be achieved by rapid cation exchange starting out from 1 b, which has not been reported for organic cations in any chalcogenido stannate salt to date.
中文翻译：
离子液体驱动的层状硫化锡酸盐的形成和阳离子交换——CH2 基团发挥作用
对简单的硫化锡酸盐K 4 [SnS 4 ]进行离子热处理，得到两种层状硫化锡酸盐或分子簇化合物。
4H 2 O 基于二元四面体 [SnS 4 ] 4−阴离子。各产物的形成，新化合物(C 4 C 1 C 1 Im) 2 [Sn 3 S 7 ] ( 1 a )、(C 4 C 1 C 2 Im) 2 [Sn 3 S 7 ] ( 1 b ) ，和(C 4 C 1 C 2 Im) 2 [Sn 4 S 9 ] ( 2 )，具有层状阴离子结构，或最近报道的化合物(C 4 C 1 C 1 Im) 4+x [Sn 10 O 4 S 16 (SMe) 4 ][An] x ( A )包含分子簇阴离子，通过离子液体阳离子的选择和反应温度两者来控制。我们报告了与其他报道的相关化合物的离子热合成相比，合成放大了 100 倍，以及如何以纯相形式分离它们的程序——这两者都是离子液体中硫族锡酸盐化学中罕见的观察结果。此外，化合物1a的合成可以通过从1b开始的快速阳离子交换来实现，迄今为止尚未报道任何硫族锡酸盐中的有机阳离子。
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