Nitrido-Bis Triphenylphosphorus

Tetrahydrofuran (THF) and diethyl ether are freshly distilled from sodium benzophenone ketyl under nitrogen. Hexane is freshly distilled from sodium metal under nitrogen. Triruthenium dodecacarbonyl is available commercially or it can be synthesized from ruthenium trichloride trihydrate (Alfa) using the procedure of Mantovani and Cenini,3a or alternately, by the procedure given in this volume.3b The [/r-nitrido-bis(triphenylphosphorus)(l+)] chloride can be purchased from Strem or synthesized according to the literature procedure4... 

The contents of the Carius tube should appear as a brown solid. This is extracted with 50-mL portions of ethyl acetate each brought to boil in the Carius tube by heating it in an oil bath under stirring. When the solvent is pale pink in color, all the neutral clusters will have been extracted. The residue contains a mixture of high nuclearity osmium anions of which [Os10C(CO)24]2- and [OsnC(CO)27]2 have been fully characterized.3 These can be extracted with a methanol-acetone (1 1) solution of [PPN]C1, (/i-nitrido-bis(triphenylphosphorus)(l +)] chloride (Ventron) and separated by fractional crystallization from acetone-methanol. 

B. BIS[ i-NITRIDO-BIS(TRIPHENYLPHOSPHORUS)(l +)] [ (DODEC AC ARBON YLPL ATINUM-TETRARHODATE(2—) ], [(Ph3P)2N]2[PtRh4(CO)12]... 

CrFeNO,P2C4jH,i, Chromate(l -)hydrido-nonacarbonyliron-, p-nitrido-bis-(triphenylphosphorus)(l +), 26 338... 

HFeNO,WC45Hm, Tungstate(l-), hydri-dononacarbonyliron-p-nitrido-bis(triphenylphosphorus)(l +), 26 336... 

NC12Hm, Pyridine, 2-(phenylmethyl)-palladium complex, 26 208-210 NCi2H,j, Naphthalenamine, /V.A -dimethyl-lithium complex, 26 154 NCi2Hv, Benzo[/i]quinoline ruthenium complex, 26 177 NCojCuO CuH, Ruthenium, (acetonitrile)-dodecacarbonyltricobaltcopper-, 26 359 NCo Oi RuC,2H2(1, Ruthenate(l-), dodeca-carbonyltricobalt-tetraethylammonium, 26 358 NCrFeOvP2C45Hji, Chromate(l-), hydri-dononacarbonyliron-(x-nitrido-bis( triphenylphosphorus)( 1 +), 26 338... 

NFejOuPiCwH, Ferrate(2-), pj-carbido-dodecacarbonyltetra-bis[ x-nitrido-bis(triphenylphosphorus)-(1+)], 26 246... 

NiOuP UjCsnH, Rulhenate(l -), tetra-decacarbonylnitridopenta-p-nitrido-bis(triphenylphosphorus)( 1 +), 26 288... 

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