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The development of molecular-biological bases of novel diagnostical radiopharmaceuticals (RP) is the comprehensive complex interdisciplinary problem of current biology, chemistry, physics and medicine. The key problem of using of RP for the positron-emission tomography (PET) is either the short radionuclide decay time or the complexity of its incorporation into the working molecule. The elaboration of easily modified ligand systems with high affinity to the metal cation as well as with wide possibilities of chemical modifications including the conjugation to the biological vectors is proposed. In this lecture we will discuss the synthetic chemistry, conformation and stability studies of two sets of novel ligands for PET – (i) piperazine-based tetraaza-macroheterocycles and (ii) the tetradentate bispidines. The data obtained are important for the study of new metal complexes including those that could be used for PET. This work was supported by Russian Science Foundation, grant 16-33-00114.