The crystal structure of bis(thioglycinato)nickel(II), Ni(C2HaNOS)2, has been determined from nearly complete three-dimensional visually estimated X-ray diffraction data collected using Cu Kct radiation, and refined by full-matrix least-squares methods to a final conventional R index of 0.139. The deep red-violet crystals have space group symmetry P2dc with ao=7"231, bo= 10"784, Co= 11.100 A, fl= 105"7 °, and with four molecules per unit cell. Two chemically similar, but crystallographically nonequivalent, molecules are found in the structure, each with a centrosymmetric square-planar arrangement of ligands about Ni(II). The geometries of these two molecules agree well. Each molecule participates in the maximum number of intermolecular hydrogen bonds. The bond lengths and angles agree well with those in similar compounds, except for the sulfur-carbon distances (1.721 _+ 0-005 A) which show appreciable multiple-bond character. Apart from the nitrogen and hydrogen atoms, each molecule is relatively planar.