Preparation of thionylimide complexes of titanium, zirconium, and hafnium. Crystal structure of [Zr(cp)(η-C5Me5)(NSO)2]

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Abstract
The compounds [Ti(cp)2(NSO)2], [Zr(cp)(η-C5Me5)2(NSO)2], [Zr(η-C5Me5)2(NSO)2], and [Hf(cp)(η-C5Me5)(NSO)2](cp =η-C5H5) have been prepared from corresponding metal halides and K(NSO). The transition-metal-bonded NSO groups can be transformed into NSNSiMe3 by reaction with Li[N(SiMe3)2], giving [Ti(cp)2(NSNSiMe3)2]. A compound containing three NSO ligands has been prepared from the reaction of SnMe3(NSO) and [Ti(cp)Cl3]. The X-ray crystal structure of [Zr(cp)(η-C5Me5)(NSO)2] reveals a pseudo-tetrahedral co-ordination of the metal, with two nitrogen-bonded NSO ligands forming a nearly planar Zr(NSO)2 unit.