Three heterometallic 1-D polymers, [{Ni(1,10-phen)(2)(H2O)}(2) {(Mo5O15)(4,4'-dbp)} (.) (5.75H(2)O)] (4,4-dbp = O3PCH2C6H4C6 H4CH2PO3) (1), [{Co(1,10-phen)(2)(H2O)}(2) {(Mo5O15)(4,4'-dbp)} (.) (5.5H(2)O)] (2) and [{Ni(2,2'-bpy)(3)} {Ni(2,2'-bpy)(2)(H2O)} {(Mo5O15)(4,4'-dbp)} (.) (4.75H(2)O)] (3), have been synthesized under hydrothermal conditions. Their structures were determined by single crystal X-ray diffraction. The 1-D chains is constructed of [Mo5O15(4,4'-dbp)](4-) units, which are further decorated and charge compensated by [M(1,10-phen)(2)] (M = Ni, Co) or [Ni(2,2'-bpy)(2)] subunits. The thermogravimetric analyses and magnetic properties of 1 and 2 were studied. (c) 2005 Elsevier Inc. All rights reserved.