Synthesis and structural characterization of an open cage dithiatungstaborane [(CpW)₂B₄H₄S₂] cluster

Abstract

Reaction of Cp^#MCl₄, (<b>1</b> or <b>2</b>) [(<b style="">1</b>): M = Mo, Cp^#= Cp* (Cp* = <img src='/image/spc_char/Etta.gif' border=0> ⁵-C₅Me₅) and (<b style="">2</b>): M = W, Cp^#= Cp (Cp = <img src='/image/spc_char/Etta.gif' border=0>⁵-C₅H₅)] with excess of [LiBH₄.thf] followed by thermolysis with excess of [HS(CH₂)_nSH] (n = 2 or 3), leads to the formation of<b style=""> </b>[(Cp*Mo)₂B₄H₄S₂] (<b style="">3</b>) or [(CpW)₂B₄H₄S₂] (<b style="">4</b>) respectively. Corresponding to (<b>3</b>) and (<b>4</b>), the compounds [(M)₂B₅H₉] (M = CpW, (<b style="">5</b>) or Cp*Mo, (<b style="">6</b>)) are isolated as major product in both the cases. These new compounds have been characterized in solution by mass, ¹H, ¹¹B, ¹³C NMR spectroscopy. The structural types have been unequivocally established by X-ray crystallographic analysis of compounds (<b style="">4</b>).