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Synthesis and Complexation of 1,2‐Bis[(monoaza[15]crown‐5)‐ N ‐yl]glyoxime. Crystal Structure of (1,2‐Bis[(monoaza[15]crown‐5)‐ N ‐yl]glyoximato)palladium(II)

1990; Wiley; Volume: 73; Issue: 1 Linguagem: Inglês

10.1002/hlca.19900730120

1522-2675

Vefa Ahsen, Emel Musluoǧlu, Ayşegül Gürek, Ahmet Gül, Özer Bekâroĝlu, Margareta Zehnder,

Metal-Catalyzed Oxygenation Mechanisms

Abstract A new vicinal dioxime ligand with two crown‐ether groups, 1,2‐bis[(monoaza[15]crown‐5)‐ N ‐Yl]‐glyoxime(LH 2 ), has been prepared from cyanogen di‐ N ‐oxide and monoaza[15]crown‐5. Ni(II), Pd(II), and Pt(IV) complexes of LH 2 with or without alkali‐metal ions bound to macrocyclic groups have been isolated. The high affinity of [Pd(LH) 2 ] and [Ni(LH) 2 ] for the K + ion is observed in solvent extraction experiments. A single‐crystal X‐ray structure confirms the postulated geometry of [Pd(LH) 2 ]‐ The Pd‐atom of the centro‐symmetric molecule has square‐planar PdN 4 coordination where Pd–N distances range from 1.978(3) to 1.970(3) Å. The N–Pd–N intraligand angle is 79.9(1) ° .