Salts of Mixed Platinum-Tetrarhodium Cluster Complexes

SALTS OF MIXED PLATINUM-TETRARHODIUM CLUSTER COMPLEXES 

Submitted by ALESSANDRO FUMAGALLI and SECONDO MARTINENGO Checked by PIERRE BRAUNSTEIN1 and DOMINIQUE WATT  

Both the products described here and the reaction intermediates are highly sensitive to oxygen, thus all the manipulations are carried out using inert atmosphere techniques4 with standard Schlenk ware. Oxygen-free carbon monoxide (purity 99.95%, 02 2 ppm) is from cylinders, and used without further purification. 

BIS [p-NITRIDO-BIS(TRIPHEN YLPHOSPHORU S) ((1 +)] [TETRADECACARBONYLPLATINUM-TETRARHODATE(2—)], [(Ph3P)2N)]2[PtRh4(CO)14] 

The compound [(Ph3P)2N]2[PtRh4(CO)14] is a yellow-orange crystalline solid that must be stored under CO. Large crystals are stable in air for a few hours, but its solutions are quickly oxidized. It is soluble in THF, acetone, and acetonitrile, sparingly soluble in methanol, and insoluble in 2-propanol, hexane, and water. The solutions are stable only under CO. Purity can be judged by the color, by analysis, and by the IR spectrum in THF solution. The solution must be prepared under CO, and the IR cells must be previously purged with CO, IR bands are observed at 2030 (vw), 1995 (s), 1962 (vs), 1941 (m,sh), 1900(vw), 1854(vw), 1807(ms), 1800 (ms, sh), and 1751 (m)cm 1. 

Standard 1M HCl. Reagents with a different Pt or Rh content, and NaOH solution with a slightly different titer may be used as well, provided that the same Pt-Rh-NaOH ratio is maintained. The [ Ph3P)2N]Cl is available from Strem. 

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Salts of Mixed Platinum-Tetrarhodium Cluster Complexes 373... 

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