The reaction of the 4-hydroxy-pyridine-2,6-dicarboxylic acid (for short H3hypydc) and 2-aminopyrimidine (for short 2-apym) with vanadiumIII and ironIII chloride in distilled water medium produces prism brown crystals of (2-apymH)[VO2(hypydc)].H2O (1) and needle colorless crystals of (2-apymH)[Fe(hypydc)2] (2), respectively. Both crystal structures were thoroughly characterized by CHN elemental analyses, FTIR spectroscopy, TGA, and SXRD methods. 1 and 2 crystallize in the space group P 1 of thetriclinic and Pbca of the orthorhombic systems, where the final R values for 1 and 2 are 0.0312 for 3641 reflections collected and 0.0315 for 5016 reflections collected, respectively. The unit cell dimensions for 1 are: a = 6.3875(4) Å, b = 7.9518(5) Å, c = 13.8489(9) Å and a = 94.9210(10)°, b= 94.4130(10)°, g = 90.3460(10)° and for 2 are a = 7.8679(3) Å, b = 16.0020(6) Å, c = 30.0965(11) Å. The VO2 + group is coordinated by two oxygen and one nitrogen atoms of the (hypydc)2– ligand and FeIII atom is coordinated by four oxygen and two nitrogen atoms of the (hypydc)2– ligand. The coordination geometry around VV and FeIII centres are distorted trigonal bipyramid and distorted octahedron, respectively.

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