A sequence of stages in the syntheses of isomeric bisamino acid complexes of Pt(II) with beta-aminopropionic acid (beta-alanine = beta-AlaH) has been studied by the (195)Pt NMR spectroscopy. The techniques have been developed of the synthesis of the cis- and trans-bischelates of Pt(II) and Pd(II) with beta-alanine as well as of the halide complexes of trans-[M(beta-AlaH)(2)Cl(2)] (M = Pt, Pd) and trans-K(2)[Pt(beta-Ala)(2)I(2)] types. The NMR spectroscopy and IR spectroscopy (in the nuclei of (195)Pt,(13)C,(1)H) and X-ray diffraction analysis have been used to examine the structures of the synthesized compounds.