Temperature Influence on the Formation of Selenidoantimonates: Solvothermal Syntheses,Crystal Structures and Thermal Properties of [Ni(dien)2]2Sb2Se6, [Mn(dien)2]2(SbSe4)(Cl), [Co(dien)2]2(SbSe4)(Br), and [Co(dien)2]3(SbSe4)2 |
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| Authors: | Qin‐yan Jin Ai‐mei Zhu Ying‐li Pan Ding‐xian Jia Dr Yong Zhang Jian‐sheng Gu |
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| Institution: | School of Chemistry and Chemical Engineering, Suzhou University (Dushu Lake Campus), No.199 Renai Road, Suzhou, 215123, P. R. China |
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| Abstract: | New selenidoantimonats Ni(dien)2]2Sb2Se6 ( 1 ), Mn(dien)2]2(SbSe4)(Cl) ( 2 ), Co(dien)2]2(SbSe4)(Br) ( 3 ), and Co(dien)2]3(SbSe4)2 ( 4 ) (dien = diethylenetriamine) were solvothermally synthesized in dien solvent at 180 °C. The crystal structure of 1 consists of two octahedral Ni(dien)2]2+ cations and a mixed‐valent Sb2Se6]4? anion. The isolated Sb2Se6]4? anion is formed by a SbIIISe3 trigonal pyramid and a SbVSe4 tetrahedron sharing a common corner. 2 and 3 are composed of octahedral M(dien)2]2+ cations, tetrahedral SbSe4]3? anions and halide ions forming an extended network through hydrogen‐bonding interactions. In 4 the Co(1)(dien)2]2+, Co(2)(dien)2]2+ and SbSe4]3? ions form layered structures via N–H···Se hydrogen bonds. The Co(3)(dien)2]2+ ion is located between the layers, and interacts with the layers by N–H···Se bonds. The synthesis and solid state structural studies on the title compounds show that the higher reaction temperature is helpful for the formation of selenidoantimonate(V) compounds in the synthesis of selenidoantimonate from the M2+/Sb/Se/dien system. 1 – 4 start to decompose at temperature about 210 °C in N2 atmosphere. They lose dien ligands at a wide temperature range of 210–450 °C with multisteps for 1 – 3 and a single step for 4 . |
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| Keywords: | Solvothermal syntheses Transition metals Selenidoantimonates Crystal structures |
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