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Journal of Structural Chemistry

2011 year, number 3

NEW Nine-Coordinate (NH4)3[YbIII(ttha)]·5H2O and Eight-Coordinate (NH4)[YbIII(pdta)(H2O)2]·5H2O Complexes: Structural Determination

J. Wang1, P. Hu1, G. Han1, L. Zhang2, D. Li1, R. Xu3, X. Chen1, X.D. Zhang1
1 Department of Chemistry, Liaoning University
2 Department of Pharmacy, Liaoning University
3 Center of Analysis and Test, Liaoning University
wangjuncomplex890@126.com
Keywords: ytterbium(III), ttha, pdta, complex, synthesis, structure
Pages: 592-598

Abstract

The (NH4)3[YbIII(ttha)]·5H2O (I) (H6ttha = triethylenetetramine-N,N,N′,N″,N′′′,N′′′-hexaacetic acid) and (NH4)[YbIII(pdta)(H2O)2]·5H2O (II) (H4pdta = propylenediamine-N,N,N′,N′-tetraacetic acid) complexes are synthesized by heat-refluxing and acidity-adjusting methods, and their structures are determined by single crystal X-ray diffraction techniques. These two complexes are all mononuclear structures. The complex I crystallizes in the monoclinic crystal system with the P21/c space group. The central YbIII ion is nine-coordinated only by one ttha ligand, and one non-coordinate carboxyl group is left. The crystal data are as follows: a = 10.321(4), b = 12.744(5), c = 23.203(9) Å, β = 91.082(6)°, V = 3051(2) Å3, Z = 4, Dc =
= 1.754 g/cm3, μ = 3.150 mm-1, F(000) = 1636, R = 0.0357, and wR = 0.0672 for 6203 observed reflections with I ≥ 2σ(I). The YbN4O5 part in the [YbIII(ttha)]3− complex anion forms
a pseudo-monocapped square antiprismatic polyhedron. The complex II is coordinated with one pdta ligand and two water molecules, which form an eight-coordinate structure, and crystallizes in the triclinic crystal system with the space group. The YbN2O6 part in the [YbIII(pdta)(H2O)2] complex anion makes a pseudo-square antiprismatic polyhedron. The crystal data are as follows: a = 9.8923(9), b = 10.9627(10), c = 12.2618(11) Å, α = 67.284(5)°, β = 70.956(6)°, γ = 68.741(5)°, V = 1115.97(18) Å3, Z = 2, Dc = 1.843 g/cm3, μ = 4.264 mm-1, F(000) = 618, R = 0.0177, and wR = 0.0409 for 4036 observed reflections with I ≥ 2σ(I).