Abstract: 2+1 tricarbonyl complexes [Re(CO)₃(N^N)CNCH₂COOEt]X, where N^N = 2,2′-bipyridine (bipy) or 1,10-phenanthroline (phen) and X = Cl^– or ClO₄^–, were prepared and isolated by two procedures. The intermediate tricarbonyl complexes [Re(CO)₃(N^N)X] (where X = Cl^– or ClO₄^–) were also isolated. The composition and molecular structure of these complexes were determined by single crystal X-ray diffraction analysis. The complexes have fac-tricarbonyl structure with bidentate coordination of bipy and phen. The complexes were characterized by PL, IR, UV-Vis, and ¹H NMR spectroscopy and by elemental analysis.