CO in tetrahydrofuran; dichloromethane all manipulations under N2 or Ar; combining (PPN)Cl and the cluster in THF, bubbling CO through the mixt., sealing (1 atm CO), stirring (93 h), removing THF (vac.), dissolving (CH2Cl2), bubbling CO through soln. (-80°C, 15 min), adding CF3SO3CH3; warming to room temp., removal of the solvent under vac., chromy. (silica gel, 1:9 CH2Cl2/hexane, first band: Os3(CO)12, second band: Os3(exo-μ2-N(H)Ph)(μ2-Cl)(CO)10, third band: product); elem. anal.;

CF3COOH in tetrahydrofuran byproducts: {N(P(C6H5)3)2}{CF3COO}; all manipulations under N2 or Ar; combining the cluster with (PPN)I, addn. of CF3COOH, stirring for ca. 12 h; removal of the solvent (vac.), chromy. (silica gel, 1:9 CH2Cl2/hexane, first band Os3(CO)12, second band Os3(exo-μ2-N(H)Ph)(μ2-I)(CO)10, third band product (recrystn. from pentane; elem. anal.), forth band Os3(endo-μ2-N(H)Ph)(μ2-I)(CO)10;