Bis triphenylphosphine dinitrosylcobalt l Tetraphenylborate

Anhydrous C0CI2 (12.0 mmoles) is prepared as in Sec. A. After the addition of 75 ml of methanol, 8.3 ml (60.0 mmoles) of NEt3 (distilled from KOH) is slowlyl added to.the solution of C0CI2. As in Sec. A, NO is bubbled through the reaction solution for 8-10 hr, and the solution is degassed. 

A solution of 7.86 g of PPhst (30.0 mmoles) in 75 ml of hot ethanol, under a strong flow of N2 using a funnel inserted in the unused neck of the flask, is quickly added to the red-brown reaction solution of [Co(NO)2Cl]2 the resulting mixture is stirred for 3 hr. A solution of 9.0 g of Na[BPh4] (26.6 mmoles) 

If the NEt3 is not carefully distilled or is added too fast, a small amount of precipitate is formed. 

Scare is required because [Co(NO)2CI]2 is very air-sensitive, especially in solution. 

The dinitrosyl cations prepared here are air-stable as dry solids but sensitive to air and water in solution all reactions and subsequent work-ups should be carried out in appropriate Schlenk glassware under prepurified nitrogen. Solubilities and NO stretching frequencies appear in Table I. 

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