Metal-organic frameworks are a class of porous polymeric material, consisting of metal ions linked together by organic bridging ligands. They are recently emerging on the interface between molecular coordination chemistry and material science.The [Ca(PYR)2], [Cu(ANTH)2] and [Zn(MAL)(PYR)] complexes were synthesized by the solvent based and solvent free methods of synthesis using a combination of solvents.Physical and analytical data of the complexes formed shows the [Ca(PYR)] complex to be whitish powder with a melting point greater than 300oC while the [Cu(ANTH)] complex synthesized by refluxing method was observed to have a melting point >400. FTIR analysis of the complexes shows thebidentate mode of coordination of the [Zn(MAL)(PYR)] and the [Cu(ANTH)], observed in the absorption bands at 469 and 501 cm-1 attributed to the ʋ(M-N) and ʋ(M-O) in the [Zn(MAL)(PYR)], and at 495 and 521 cm-1 in the [Cu(ANTH)] synthesized by the solvent based method while the ʋ(M-N) and ʋ(M-O) bands for the [Cu(ANTH)] prepared by solvent free method of synthesis was observed at 484 and 515 cm-1 . FTIR analysis results of the complexes synthesized by the solvent free method showed close similarity with the FTIR spectra of the complexes synthesized by the solvent based method. The complexes were observed to be stable up to a temperature of about 300oC.