The synthesis and self-assembly of Silver (I) and Cobalt (II) with the 4-pyridylthioacetate (pyta) ligand leads to two new coordination polymers, Ag(pyta) ( 1) and [Co(pyta) 2H 2O] ( 2). 1 is a three-connected silver coordination polymer, which consists of a wave layer and regular rectangle cavities (5.54×8.16 Å). While 2 is constructed by fascinating assembly of pyta ligands with a new structure of seven-coordinate cobalt ions. The two-dimensional layers structure is based on four kinds of chiral helices viewed from a and b directions. The crystallographic parameters are as follows: for 1, monoclinic, space group P21/ c, with a=8.160(2) Å, b=10.109(2) Å, c=10.097(2) Å, β=104.93°, and Z=4; for 2, monoclinic, space group C2/ c, a=15.928(3) Å, b=6.3448(12) Å, c=15.582(3) Å, β=94.698(3)°, and Z=8.