Two hexanuclear molybdophosphonates, Na2H4{(CH3COO)[N(CH2PO3)3]Mo6O17(OH)}·13H2O (1) and Na2(NH4)4[Mn2Na2(H2O)2]{[HN(CH2PO3)2](CH3COO)PMo6O22}2·16H2O (2), have been successfully synthesized and characterized by X-ray crystallography, elemental analysis, IR spectra and XRPD, along with a 31P NMR spectroscopic study for 1 and a magnetic susceptibility study for 2. Compounds 1 and 2 are prepared in solution by the self-assembly of the amino trimethylene phosphonic acid (noted as ATMP) ligand and heptamolybdate. Compound 1 exhibits a ring-shaped cluster with two branches of the ligand bound off-center, while the introduction of Mn ions breaks the central P–C bond to form a dinuclear Mn(II) sandwich-type polyanion 2. The magnetic susceptibility of 2 shows strong antiferromagnetic interactions between the two MnII cores.
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