Three novel transition metal complexes with 1,3,5-benzenetricarboxylic acid, H(3)btc, and 2,2 -bipyridine have been obtained through hydrothermal method and their crystal structures were determined by X-ray diffraction. Complex [Ni-2(bpy)(btc)(OH)](n) (1) crystallizes in the monoclinic space group P2(1)/n, with a = 10.1457(3), b = 11.7643(3), c = 16.9973(3) Angstrom, beta = 98.747(1)degrees and Z = 4. Complex [Co-2(bpy)(btc)(OH)](n) (2), which is isomorphous to 1, crystallizes in the monoclinic space group P2(1)/n too, with a = 10.152(6), b = 11.828(3), c = 17.107(6) Angstrom, beta = 98.700(3)degrees and Z = 4. 1 and 2 contain double-stranded chains connected by btc(3-) ions in different directions to form 3D networks. {[CO1.5(bpy)(btc)].(H2O)(2)}(n) (3) crystallizes in monoclinic space group C2/c, with a = 15.2478(3), b = 15.2007(6), c = 16.5168(5) Angstrom,beta = 110.111(1)degrees and Z = 8. 3 consists of two-dimensional sheets containing three types of rings and the sheets are connected by btc(3-) ligands to create a compact 3D network. (C) 2003 Elsevier B.V. All rights reserved.