The reaction of 2,4-bis (4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane-2,4-disulfide (Lawesson(')s reagent) with phenylethylamine produced [H3NCH2CH2C6H5](+) [(C6H5CH2CH2NH)(p C6H4OMe)PS2](-) (1). Furthermore, reaction of 1 with NiCl2 in dry methanol led to the novel complex 2. The compounds were characterized by H-1 and P-31 NMR, IR spectroscopy, and elemental analysis. A single crystal X-ray structure of complex 2 showed that the nickel complex is square planar. The complex formed a supramolecular structure via intermolecular S1...H7B and O1...H2N2 hydrogen bonds. The X-ray crystallography of complex showed [R-2(2)](18) and R-4(4)(18) motifs in the monomers were connected to each other via S1...H7B, O1...H2N2 hydrogen bonds with donor-acceptor distance of 2.89 and 2.51 angstrom, respectively. The new compounds were additionally tested in view of their antibacterial properties.[GRAPHICS].