Reactivity of molecules containing element-element bonds. 2. Transition elements [Erratum to document cited in CA114(15):143614m] (original) (raw)

was done by extraction with THF (20 mL) followed by vacuum drying, dissolution in water (10 mL) and addition of NaCl (20% w/v, 7.5 mL), and, after overnight standing, filtration of a small precipitated impurity, followed by cautiously layering on the clear solution of CsCl (3% w/v, 20 mL). After complete diffusion (several weeks), the precipitated pure C S~[ P~~R~~~( C O ) ~~] was filtered and washed with CsCl (3% w/v, 10 mL). The clear mother liquor and collected washings were treated with CH3COOH (4 mL) to give after about 3 h a fine crystalline precipitate. After the mixture was allowed to stand overnight, C S~[ P~~R~~~( C O )~~] was separated from the mother liquor by decantation and vacuum dried. Yields: 100-150 mg (3-4%). The product gave no hydrido signals in 'H NMR. (b) Synthesis as a Byproduct of the Synthesis of [F'tzRh~(CO)zz]3-. [PPN][PtRh5(CO)15] (1.143 g, 0.685 "01)