Anionic and Heteronuclear Triosmium Clusters

Submitted by KEVIN BURGESS and ROSS P. WHITE Checked by RICHARD D. ADAMS aad JAMES E. BABIN 

The relatively stable polymetallic Os3(CO)i2 (ref. 6) may be activated by conversion to anionic derivatives. Reduction of Os3(CO)j2 with potassium benzophenone gives the reactive, air-sensitive triosmium dianion [Osj(CO)i, ] . Generally, it is convenient to generate and use this complex immediately, without isolation Section B describes an example of this procedure 

PH0SPHINE)G0LD]TR10SMIUM AND DECACARBONYL-fi-HYDRIDO-n-[(TRlETHYLPHOSPHlNE)GOLD]TRIOSMIUM 

Decacarbonyl-/i-hydrido-/i-[(triethylphosphine)gold]triosmium is prepared in the same way from 0.042 g (0.12 mmol) of Au(PEt3)Cl, giving a green band rf = 0.4 (solvent as above) 0.059 g (51% yield) before 

Decacarbonyl- -hydrido-/i-[(triethylphosphine)gold]triosmium has similar properties and spectral characteristics. IR (hexane cm ) 2089(m), 2045(s), 2039(m), 2008(s), 1995(s), 1978(s), and 1943(vw). The HNMR spectrum (250 MHz, chloroform-d, 5 parts per million downfield from TMS, ambient temperature) shows a doublet of triplets (J= 19 and 9 Hz) at 1.15 resulting from the methyl hydrogen atoms, a multiplet at 1.85 for the methylene protons, and a sharp hydride singlet at — 11.84. Low resolution mass spectra of this compound contain a peak at m/z = 1172 corresponding to the molecular ion ( Os, Au). 

PHOSPHINE)GOLD]TRIOSMIUM AND DECACARBONYL-p-HYDRIDO-p-[(TRIETHYLPHOSPHlNE)GOLD]TRIOSMIUM 

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