1,2-Ethanediyliden)-bis(S-methylhydrazonecarbodithionate) ligands 1a-g form zinc chelates with [ZnN 2 S 2 ] units, as shown by means of IR, NMR, XPS, X-ray crystal structure analysis, and Zn and N K-edge XANES. The conformation of ligands 1a-g strongly determines the structure of the corresponding zinc complexes 2a-g. Powder samples of these complexes were studied by Zn K-edge XANES. The Zn K-edge XANES results agree with those of X-ray crystal structure data, when available. A tetrahedral ligand environment was confirmed for only one complex (2a). The other zinc chelates (2b-g) show dimeric structures with square pyramidal complex geometry. With pyridine, five-coordinated zinc complexes 3a-c form, as shown by Zn K-edge XANES in comparison with X-ray crystal structure data. XANES studies afford considerable advantage for obtaining structural information, in particular when crystals of sufficient quality cannot readily be obtained.
Die dreizähnigen Liganden S‐Methyl‐β‐N‐(2‐hydroxyphenyl)‐methyliden‐ (H2Sal) und S‐Methyl‐β‐N‐(2‐pyridyl)‐methyliden‐dithiocarbazon (HPyr) reagieren in unterschiedlicher Weise mit Diorganozinn(lV)‐oxiden. Mit dem erstgenannten Liganden zu dem fünffach koordinierten Komplex R2SnSal mit trigonal bipyramidaler Struktur, in der Reaktion mit dem zweiten Liganden zu dem Zweikernkomplex [(R2SnPyr)2CO3] mit einem Carbonatanion als Brückenligand. Die Strukturaufklärungen erfolgten mittels Röntgenkristallstrukturanalyse und in Lösung mit multinuklearer NMR‐Spektroskopie. IR‐ und massenspektrometrische Messungen ergänzen die Aussagen.
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