Bis tetrafluoroammonium Hexafluoromanganate IV

The same apparatus is used as for synthesis C. In the dry Nj atmosphere of a glove box, a mixture of [NF4][SbFft] (37.29 mmol) and CsjlMnF ] (18.53 mmol) is placed in the bottom of a prepassivated (with CIF3) Teflon FEP (flu-oroethylene propylene copolymer) double U-tube metathesis apparatus. Dry HF (20 mL of liquid) is added at -78° on the vacuum line, and the mixture is warmed to 25° for 30 min with stirring. The mixture is cooled to -78° and 

Bis(tetrafiuoroammonium) hexafiuoromanganate(IV) is a yellow crystalline solid that is stable at 65° but slowly decomposes at 1(X)° to NFj, Fj, and MnFj. It is highly soluble in anhydrous HF and reacts violently with water. Its F NMR spectrum in anhydrous HF solution shows a broad resonance at ( 218 ppm below CFClj due to [NF4]. The vibrational spectra of the solid show the following major bands IR (pressed AgCI disk) 1221 (mw), 1160 (vs), 620 (vs), and 338 (s) cm . Raman 855 (m), 593 (vs), 505 (m), 450 (w), and 304 (s) cm  

25° for 14 hr. The materials volatile at 25° are pumped off again. They contain less than 1 mmol of HP at this point. The solid residue is heated in a dynamic vacuum to 50° for 28 hr or until no further HP evolution is noticeable. The white solid residue (about 3.8 g, 80% yield) has the approximate composition (weight %) [NP4]j[SiP6] 95.0, Cs[SbPJ 2.2, [NP llShP,.] 2.3. 

A solution of 20 mmol of [Np4][Hp2] in 16 mL of dry HP is prepared at —78° by synthesis C and pressure-filtered into the second half of the metathesis double U-tube containing 14.6 mmol of WOp4. The mixture is stirred with a magnetic stirring bar for 30 min at 25°. The volatile material is pumped off at 25° for 12 hr. The solid residue (about 5 g, 86% yield based on WOP4) has the approximate composition (weight %) [NP4KWOP5] 96, Cs[SbPs] 2, [Np4][SbPe] 2. 

Inorganic Syntheses, Volume 24 Edited by Jean ne M. Shreeve 1986 by Inorganic Syntheses, bic. 

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