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Hydrothermal synthesis of a mixed-valence hexamolybdate cluster: crystal structure of [HN(CH2CH2)3N]2[HMoVMoVI5O19]·[N(CH2CH2)3N]

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Abstract

The hydrothermal reaction of MoO3, V, Na2WO4· 2H2O, [N(CH2CH2)3N](1,4-diazabicyclo[2.2.2] octane), and H2O at 160°C for 90h gave dark-brown crystals of [HN(CH2CH2)3N]2[HMoVMoVI 5O19]·[N(CH2CH2)3N], (1), in 40% yield. Complex (1) is the first one-electron reduced mixed-valence hexamolybdate to be crystallized and structurally characterized. The crystal structure of (1) consists of discrete [HMoVMoVI 5O19]2− anions, [HN-(CH2CH2)3N]+ cations, and neutral [N(CH2CH2)3N] molecules of crystallization.

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Khan, M.I., Cevik, S. & Powell, D. Hydrothermal synthesis of a mixed-valence hexamolybdate cluster: crystal structure of [HN(CH2CH2)3N]2[HMoVMoVI5O19]·[N(CH2CH2)3N]. Transition Metal Chemistry 24, 436–439 (1999). https://doi.org/10.1023/A:1006973821956

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