Journal of Synthetic Crystals, Volume. 50, Issue 1, 106(2021)
Synthesis, Single Crystal Transformation and Thermal Stability of Chiral Dysprosium (III)-Tartaric Acid Complex
The new complex [Dy(Htar)3(H2O)3]n(1) was synthesized by the single crystal to single crystal transformation method using(+)-di-p-toluoyl-D-tartaric acid (D-H2DTTA) as raw material and reaction with mentalic Dy(III) salt. The complex was characterized by elemental analysis, IR spectroscopy, single crystal X-ray diffraction, powder X-ray diffraction analysis and thermogravimetric analysis and differential thermal analysis(TGA-DTA). The results of X-ray crystallographic analysis indicate that complex 1 belongs to trigonal system, space group R3 with a=b=2.723 16(14) nm, c=0.762 75(6) nm, α=β=90.00°, γ=120.00°, V=4.898 5 (6) nm3, Z=3, and Cambridge Crystallographic Data Centre (CCDC) number is 1498504. Each Dy3+ is surrounded by six O atoms from three Htar- ligands and three O atoms from three coordinated water molecules, forming a tricapped trigonal prism geometry with nine coordination property. Complex 1 exhibits an infinite one dimensional chain structure connected by O1 and O5 along c axis, with the Dy…Dy distance of 0.762 8(1) nm. Complex 1 was obtained through single crystal to single crystal transformation process from [Dy(HDTTA)3(CH3OH)3]n, which includes ester hydrolysis and water molecules substitution two reactions. Complex 1 has a certain thermal stability. After taking off the coordinated water molecules in the range of 45~166 ℃, the skeleton of 1 begins to collapse with increasing temperature above 166 ℃.
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LI Li, ZHENG Jianfeng, ZHAO Mingxia, FENG Sisi. Synthesis, Single Crystal Transformation and Thermal Stability of Chiral Dysprosium (III)-Tartaric Acid Complex[J]. Journal of Synthetic Crystals, 2021, 50(1): 106
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Received: Sep. 9, 2020
Accepted: --
Published Online: Apr. 15, 2021
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