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Using chain-like polyethers consisting of two terminal –NH2 groups and (TBA)4[α-Mo8O26] as starting materials, two polyoxometalatocrown ethers were prepared by a cyclization reaction through the formation of Mo≡N triple bonds: (TBA)2[Mo6O17N(o-C6H4OCH2(CH2OCH2)nCH2OC6H4-o)N] (compounds 1, n = 1; 2, n = 2). As confirmed by single-crystal X-ray diffraction and infrared (IR) studies, the polyoxometalatocrown ether 2 can capture primary ammonium cations in solid state.

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