Two novel rare earth metal coordination complexes, (EnH 2 )[Yb III (Egta)(H 2 O)] 2 ⋅ 6H 2 O (I) and [Yb III (Eg3a)(H 2 O) 2 ] ⋅ 6H 2 O (II), where En = ethylenediamine, H 4 Egta = ethyleneglycol bis (2 aminoeth ylether) N,N,N',N' tetraacetic acid and H 3 Eg3a = ethyleneglycol bis (2 aminoethylether) N,N,N' triace tic acid, have been successfully synthesized through direct heating reflux and natural transformation. Com plexes I, II were characterized by single crystal X ray diffraction techniques (CIF files CCDC nos. 966211 (I) and 966210 (II)). X ray diffraction reveals that I is a nine coordinate structure with a monocapped square antiprism crystallizing in the monoclinic crystal system with P2 1 /c space group. The cell dimensionsare: a = 12.9616(14) Å, b = 12.7134(13) Å, c = 15.0132(15) Å, β = 105.3720(10)° and V = 2385.5(4) Å 3 . Complex II is also mononuclear nine coordinate and crystallizes in the monoclinic crystal system with space group P2 1 /c. The cell dimensions are as follows: a = 9.1926(10), b = 10.0046(12), c = 23.536(2) Å, β = 98.9650(10)°a nd V = 2385.5(4) Å 3 . However, when I is continued to direct heating reflux, the octadentate Egta ligand losts an acetic acid group and becomes a heptadentate Eg3a ligand. Thus, II was obtained, which was confirmed by means of single crystal X ray diffraction analysis. This finding may offer a fast and efficient one step reac tion synthesis method of asymmetric aminopolycarboxylic acid.