Abstract

The role of borate anions in ionothermal syntheses of crystalline chalcogenidometalates was shown by the directed ionothermal synthesis of seven new selenidostannates in ionic liquids with either [BF4 ]- or [B(CN)4 ]- anions. Single crystal structures are presented of four compounds, (C4 C1 C1 Im)5 [Sn9 Se20 ][BF4 ] (1, Im=imidazolium), (DMMPH)4 [Sn2 Se6 ] (2, DMMP=2,6-dimethylmorpholine), (C2 C1 Im)2 (DMMPH)2 [Sn6 Se14 ] (3), and K2 [Sn3 Se7 ] (4), and how the chosen ionic liquid anion, and the reaction temperature, influences the product spectrum is discussed: Notably, 1 contains an entire formula unit of the ionic liquid, (C4 C1 C1 Im)[BF4 ], while 4 contains neither the cation nor the anion of the ionic liquid-both observations being very uncommon for ionothermal syntheses. Three further compounds were obtained that exhibit strong disorder in the crystal structures (I-III), for which only their anionic substructures are discussed herein. Compound 4 and I-III are based on the same layered selenidostannate substructure, 2D-{[Sn3 Se7 ]2- }, yet with different inter-layer distances, which is clearly reflected in the crystal colors and quantitative optical absorption properties.

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