Synthesis and molecular structure oftrans-Pd(SH)2{P(i-Bu)3}2

Authors :: Ghilardi, Carlo A.
Midollini, Stefano
Nuzzi, Francesco
Orlandini, Annabella
Source :: Transition Metal Chemistry; April 1983, Vol. 8 Issue: 2 p73-75, 3p
Publication Year :: 1983
Abstract: Summary Reactions of H<subscript>2</subscript>S with [Pd(CH<subscript>3</subscript>CN)<subscript>4</subscript>](ClO<subscript>4</subscript>)<subscript>2</subscript> and PR<subscript>3</subscript> (R= Et ori-Bu) give the trinuclear thiocluster [Pd<subscript>3</subscript>(µ<subscript>3</subscript>-S)<subscript>2</subscript>(PEt<subscript>3</subscript>)<subscript>6</subscript>] (ClO<subscript>4</subscript>)<subscript>2</subscript> and the di(hydrogensulfido)-complextrans-Pd (SH)<subscript>2</subscript>{P(i-Bu)<subscript>3</subscript>}<subscript>2</subscript>, respectively. The structure of the latter compound has been determined from three-dimensional x-ray data, collected by counter methods. The crystals are monoclinic, space group P2<subscript>1</subscript>/a, with a=13.226(8), b=12.536(8), c=9.545(6) Å, ß=99.78(4)° and Z=2. Full-matrix least-squares refinements converged at the R and R<subscript>w</subscript> factor values of 0.052 and 0.054, respectively, for 2329 observed reflections. The complex shows a square planar geometry with two phosphines and two mercapto-ligands intrans configuration.