Studies On Rare-Earth Complexes with Crown Ethers. Part XXV. Synthesis, characterization, and structure of the complexes of lanthanide nitrates with 13-crown-4

✍ Scribed by Tongbu Lu; Xin Wang; Minyu Tan; Yu Liu; Yoshihisa Inoue; Tadao Hakushi

• Publisher: John Wiley and Sons
• Year: 1993
• Tongue: German
• Weight: 370 KB
• Volume: 76
• Category: Article
• ISSN: 0018-019X
• DOI: 10.1002/hlca.19930760117

✦ Synopsis

The lanthanide nitrate complexes with 13-crown-4(13-C-4) have been prepared in AcOEt. These new complexes with the general formula Ln(N03),.(13-C-4) (Ln = La-Nd, Sm-Lu) have been characterized by means of elemental analysis, IR and 'H-NMR spectra, conductivity measurements, and TG-DTA techniques. The crystal and molecular structure of Nd(N03),.(13-C-4) has been determined by single crystal X-ray diffraction. It crystallizes in the monoclinic space group P2,/a with Z = 8. Lattice parameters are Q = 15.393(1), b = 12.578(1), c = 19.279(2) A, p = 31.0 cm-'(MoK,), F(000) = 2056. The structure was solved by Patterson and Fourier techniques and refined by least-squares to a final conventional R value of 0.032 for 5218 independent reflections with I 30(2). There are two independent Experimental. -Reagents. Hydrated lanthanide nitrates were prepared by dissolving the corresponding oxides (Analu R ) in 1:l HNO,. The ligand was prepared as reported in [l]. All other chemicals used were of Analu R grade.

I) The systematic name is 1,4,7,10-tetraoxacyclotridecane.