Starting from Cu(II) and Ni(II) perchlorate and Fe(III) chloride in the presence of 2,6-diacetylpyridine (dap) and semioxamazide (sox), the [Cu(Hdapsox)H
2O]ClO
4 (I), [Ni(Hdapsox)(MeOH)
2]ClO
4 (II) and [Fe(Hdapsox)Cl
2] ·
12– H
2O (III) complexes with a singly deprotonated ligand Hdapsox
− of the acyl
hydrazone class (with H
2dapsox=2′,2
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-(2,6-pyridindiyldiethylidene)dioxamohydrazide) have been obtained and characterized for the first time by a template synthesis. The previously assumed square-pyramidal structure of the Cu(II) complex with an
asymmetrical coordination of Hdapsox
− has been confirmed by a single-crystal X-ray analysis. In II Hdapsox
− is octahedrally coordinated around a Ni(II) ion, while III is found to be a pentagonal-bipyramidal complex with a symmetrically bonded Hdapsox
−. Causes of a ligand deprotonation occurring in a very acid medium (pH=0) and of a different coordination pattern in the case of Cu(II), Ni(II) and Fe(III) are interpreted by a d
n configuration and an effective nuclear charge of the central metal ion (crystal field effects).