Hydrothermal synthesis and structure of a two-dimensional bimetallic copper–molybdophosphonate, [{Cu4(H2O)2(phenbisterpy)2(HO3P(CH2)4PO3H)}(Mo4FO12)2{O3P(CH2)4PO3}]·4H2O, constructed from {Mo4FO12}1− clusters and copper-ligand chains (phenbisterpy = 1,4-b

The hydrothermal reaction of Cu(CH3CO2)2·H2O, MoO3, 1,4-bis(2,2′:6′,2″-terpyridin-4′-yl)benzene (phenbisterpy), 1,4-butylenediphosphonic acid and HF yielded green crystals of [{Cu4(H2O)2(phenbisterpy)2(HO3P(CH2)4PO3H)}(Mo4FO12)2{O3P(CH2)4PO3}]·4H2O (1·4H2O). The structure of 1·4H2O is two-dimensional, with the network constructed from image chains and [(Mo4FO12)2{O3P(CH2)4PO3}]6− clusters. The latter building block contains two tetranuclear clusters of face- and edge-sharing {MoO5F} octahedra, linked through the diphosphonate ligand. The oxyfluoromolybdate cluster {Mo4FO12}− is structurally distinct from the few examples of tetranuclear {Mo4O12Fx}n− clusters, {Mo4O12F2}2− and {Mo4O12F3}3−.