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Articles

Syntheses, structural determination, and binding studies of nine-coordinate mononuclear (mnH)2[DyIII(Httha)]·3H2O and (enH2)3[DyIII(ttha)]2·9H2O

, , , , &
Pages 367-378 | Received 14 Jan 2012, Accepted 11 Oct 2012, Published online: 29 Jan 2013
 

Abstract

Two dysprosium coordination compounds, (mnH)2[DyIII(Httha)]·3H2O (1) (H6ttha = triethylenetetramine-N,N,N′,N″,N′′′,N′′′-hexaacetic acid and mn = methylamine) and (enH2)3[DyIII(ttha)]2·9H2O (2) (en = ethylenediamine), were synthesized through direct heating and characterized by elemental analysis, FT-IR, thermal analysis, and single-crystal X-ray diffraction. X-ray diffraction analysis displays that 1 is a mononuclear nine-coordinate complex with a pseudo-monocapped square antiprismatic conformation (MCSAP) crystallizing in the monoclinic crystal system with P2(1)/c space group. The crystal data are as follows: a = 16.1363(19) Å, b = 13.9336(11) Å, c = 13.6619(14) Å, β = 102.2490(10)°, and V = 3001.8(5) Å3. There are two kinds of methylamine cation in 1. They connect [DyIII(Httha)]2−and crystal waters through hydrogen bonds, leading to formation of a 2-D ladder-like layer structure. The polymeric 2 also is a nine-coordinate structure with a pseudo-MCSAP crystallizing in the monoclinic crystal system with P2/c space group. The cell dimensions are: a = 17.7801(16) Å, b = 9.7035(10) Å, c = 22.096(2) Å, β = 118.874(2)°, and V = 3338.3(6) Å3. In 2 there are also two types of ethylenediamine cations. One connects three adjacent [DyIII(ttha)]3− complex anions through hydrogen bonds and the other is symmetrical forming hydrogen bonds with two neighboring [DyIII(ttha)]3− complex anions. These hydrogen bonds result in formation of a 2-D ladder-like layer structure as well.

Acknowledgments

The authors greatly acknowledge the National Natural Science Foundation of China, Liaoning Province, Natural Science Foundation of Education Department, Liaoning Province, Natural Science Foundation of Science and Technology Department and Liaoning University “211” project for financial support. The authors also thank our colleagues and other students for their participation in this work. Especially, we thank Professor K. Miyoshi and T. Mizuta (Faculty of Science, Hiroshima University, Japan) for instruction.

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