4.3 Article

Syntheses and structural determinations of the nine-coordinate rare earth metal: Na-4[Dy-III(dtpa)(H2O)](2)center dot 16H(2)O, Na[Dy-III(edta)(H2O)(3)]center dot 3.25H(2)O and Na-3[Dy-III(nta)(2)(H2O)]center dot 5.5H(2)O

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JOURNAL OF COORDINATION CHEMISTRY
卷 60, 期 20, 页码 2221-2241

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TAYLOR & FRANCIS LTD
DOI: 10.1080/00958970701258622

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Three complexes, Na-4[Dy-III(dtpa)(H2O)](2).16H(2)O, Na[Dy-III(edta)(H2O)(3)].3.25H(2)O and Na-3[Dy-III(nta)(2)(H2O)].5.5H(2)O, have been synthesized in aqueous solution and characterized by FT-IR, elemental analyses, TG-DTA and single-crystal X-ray diffraction. Na-4[Dy-III(dtpa)(H2O)](2).16H(2)O crystallizes in the monoclinic system with P2(1)/n space group, a=18.158(10)angstrom, b=14.968(9)angstrom, c=20.769(12)angstrom, beta=108.552(9)degrees, V=5351(5)angstrom(3), Z=4, M=1517.87 g mol(-1), D-c=1.879 g cm(-3), mu=2.914mm(-1), F(000)=3032, and its structure is refined to R-1(F)= 0.0500 for 9384 observed reflections [I > 2 sigma(I)]. Na[Dy-III(edta)(H2O)(3)]. 3.25H(2)O crystallizes in the orthorhombic system with Fdd2 space group, a=19.338(7) angstrom, b=35.378(13)angstrom, c=12.137(5) angstrom, beta= 90 degrees, V=8303(5) angstrom(3), Z=16, M= 586.31 g mol(-1), D-c= 1.876 g cm(-3), mu= 3.690mm(-1), F(000)=4632, and its structure is refined to R-1(F)=0.0307 for 4027 observed reflections [I > 2 sigma(I)]. Na-3[Dy-III(nta)(2)(H2O)].5.5H(2)O crystallizes in the orthorhombic system with Pccn space group, a=15.964(12) angstrom, b= 19.665(15) angstrom, c=14.552(11) angstrom, beta= 90 degrees, V=4568(6) angstrom(3), Z=8, M=724.81 g mol(-1), D-c= 2.102 g cm(-3), mu=3.422mm(-1), F(000)=2848, and its structure is refined to R-1(F)= 0.0449 for 4033 observed reflections [I > 2 sigma(I)]. The coordination polyhedra are tricapped trigonal prism for Na-4[Dy-III(dtpa)(H2O)](2).16H(2)O and Na-3[Dy-III(nta)(2)(H2O)].5.5H(2)O, but monocapped square antiprism for Na[Dy-III(edta)(H2O)(3)].3.25H(2)O. The crystal structures of these three complexes are completely different from one another. The three-dimensional geometries of three polymers are 3-D layer-shaped structure for Na-4[Dy-III(dtpa)(H2O)](2).16H(2)O, 1-D zigzag type structure for Na[Dy-III(edta)(H2O)(3)].3.25H(2)O and a 2-D parallelogram for Na-3[Dy-III(nta)(2)(H2O)]. 5.5H(2)O. According to thermal analyses, the collapsing temperatures are 356 degrees C for Na-4[Dy-III(dtpa)(H2O)](2).16H(2)O, 371 degrees C for Na[Dy-III(edta)(H2O)(3)].3.25H(2)O and 387 degrees C for Na-3[Dy-III(nta)(2)(H2O)].5.5H(2)O, which indicates that their crystal structures are very stable.

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