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The crystal and molecular structure of [Cu(ampf)(ClO ₄ )(MeOH) ₂ ]ClO ₄ , (1), ampf = N,N′-bis(4-acetyl-5- methylpyrazol-3-yl)formamidine, determined by X-ray crystallography is described and compared with the structurally related copper(II) complexes, formed under similar experimental conditions, using Cu ^II salts with different anions. The complex formation is discussed in view of the structures of cobalt(II) and nickel(II) complexes with the same organic ligand and different anions, also formed under similar reaction conditions. Solvent molecules coordinated to the central atom play an important role in biologic systems. To get a better insight into the desolvation mechanism, in this study the desolvation pattern of 1 is presented. As in literature little attention is paid to the desolvation mechanism of solvate complexes, the desolvation mechanism of three, potentially biologically active isostructural pairs of octahedral Ni ^II and Co ^II compounds with ampf and dmpc (3,5-dimethyl-1H-pyrazole-1-carboxamidine) ligands are evaluated and compared with the desolvation of 1. The results of the thermal data are discussed on the basis of structural features of the compounds. The minor differences in structures of the related compounds cannot be straightforwardly connected with the different solvent evaporation mechanism. To explain the differences found in desolvation pattern in isostructural Co ^II and Ni ^II complexes the Jahn-Teller effect is proposed. © 2013 Springer Science+Business Media New York.