Dicompartmental non-macrocyclic ligands containing six (N4O2) and four (N2O2) coordination atoms were prepared. The ligands were constructed in order to investigate the effect of an opened four- oordination site (non-marcocyclic effect) on the geometrical structure of a complex in a six-coordination site with a labile metal. In this regard, monometallic non-macrocyclic complexes of Zn(II), Co(II), and Co(III) were prepared and characterized. The preparation of a Co(III) complex through two different routes, and also the X-ray crystal structure of a Zn(II) complex demonstrated that the structures of the complexes were intact even in the presence of two bulky phenyl groups in four-coordination site. The characterization of the prepared complexes confirmed the presence of two protons in the four-coordination siteof diimine complexes and a lack of them in diamine complexes.
