Ammonium hexafluorophosphate

Ammonium hexafluorophosphate [16941-11-0] M 163.0, d 2.181, pK j 0.5, pKj 5.12 (for fluorophosphoric acid H2PO3F). Crystallises from H2O in square plates. Decomposes on heating before melting. Soluble in H2O at 20° (74.8% w/v), also very soluble in Mc2CO, MeOH, EtOH and MeOAc and is decomposed by boiling acids. [Chem Ber 63 1063 1930.]... 

Cyclization takes place when tert-butylisocyanide, benzaldehyde, anilinium chloride, and carbonyl(dicyano)cyclopentadienyl ferrate are reacted, the carbene complex 42 being the result (95JOM(491)135). /50-butyraldehyde, tert-butyl isocyanide, ammonium hexafluorophosphate, and [(T -Cp)Fe(CO)(CN)2] give the cationic bis-carbene 43. 

The N-coordinated compound [AuCljL] (L= l-ethyl-2-phenylimidazole) with silver tetrafluoroborate gives the cycloaurated species 102, which on further reaction with triphenylphosphine and sodium tetrafluoroborate or ammonium hexafluorophosphate forms the cationic complexes 103 (X = BF., PF,) (00JCS(D)271). 

Pyridinedicarboxaldehyde (37) and tetraethyleneglycol bis(2-aminophe-nyl)ether (38) react to form macrocycle 39. NMR studies indicate that the three components in this mixture are in equilibrium since the imino groups, water and aldehydo/amino groups are constantly interconverting. Addition of bis(3,5-dimethoxybenzyl)ammonium hexafluorophosphate (40) species has a... 

Bis(diphenylphosphino)pyridine forms tetranuclear 111 (L = CO, S02) (83JA6332), and the carbonyl complex on interaction with carbon monoxide and ammonium hexafluorophosphate in chloroform produces [Rh2(g-L)2(CO)2(MeOH)Cl](PF6) (83JA6986). [RhAu(g-L)2](BF4)(N03)... 

The condensation of l,l -bis(chlorocarbonyl)-cobalticinium chloride (82) with various phenols and alcohols followed by chromatographic purification and excess ammonium hexafluorophosphate gave the ester-linked polycobalticinium macrocycles (83)-(86) (Scheme 28). The first... 

The solution becomes orange-red, and gas is evolved. Meth-anesulfonic acid is added to keep the pH at 2 to 3. The solution is allowed to stand, with additions of methanesulfonic acid to keep the pH at 2 to 3, until the solution becomes yellow. Solid sodium chloride is added until precipitation of [Ru(NH8)6N2]Cl2 is complete. The crude product is removed by filtration, washed with alcohol and acetone, and air-dried. It is recrystallized by dissolving in water, filtering the solution, and reprecipitating the product with solid sodium chloride. Two recrystallizations by this method yield a product which is almost white (very pale yellow). The other salts are prepared by dissolving the purified chloride salt in water and adding saturated, filtered solutions of potassium iodide or bromide, sodium tetrafluoroborate, or ammonium hexafluorophosphate until precipitation of the desired salt is complete. The products are collected by filtration, washed with a little water, alcohol, and acetone, and then air-dried. Yield is 0.5 g., 33% for the pale yellow iodide salt. Anal. Calcd. for [Ru(NH8)8N2]l2 NH, 18.19 N , 5.98 I, 54.27. Found NH8, 18.04 N, 5.35 I, 54.05. 

A 275-mg. (1-mmole) sample of C5H6Fe(CO)2Br is dissolved in 20 ml. of dry cyclohexene. After addition of 800 mg. (3 mmoles) of AlBr3, the red reaction mixture is stirred at room temperature for 4 hours. A red viscous oil is formed quite rapidly, and after 4 hours the solution is almost colorless. The colorless cyclohexene layer is decanted and the residue dried under high vacuum. About 20 ml. of ice-cold water is added while cooling with ice, and the orange solution is filtered into an excess of a concentrated solution of ammonium hexafluorophosphate. The precipitate is collected and dried under high vacuum. For further purification, the yellow salt is dissolved in 10 ml. of acetone, and, after filtration, ether is added drop-wise until no more precipitate separates. After a second crystallization, the product is obtained in about 40% yield, based on C8H5Fe(CO)2Br. Anal. Calcd. C, 38.64 H, 3.74 F, 28.21 Fe, 13.8 P, 7.67. Found C, 38.55 H, 3.75 F, 28.6 Fe, 13.8 P, 7.43. 

The salt is easily converted to the water-insoluble hexafluoro-phosphate. A filtered solution of 0.766 g. of the crude salt in 15 ml. of water is precipitated by slowly adding excess saturated aqueous ammonium hexafluorophosphate while the solution is stirred. The filtered solid is washed (50 ml. of water) until free of bromide ion and then washed with 30 ml. of anhydrous diethyl ether. Yield of the dried product is 0.973 g. (96%), m.p. 248-250°C. Recrystallization by letting a warm solution (20 ml. of 1 1 water-acetone) evaporate slowly gives no change in melting point. 

The interaction of an alkyne with (tj5-C5H5)(PR3)2RuX can result in the formation of a wide variety of ruthenium complexes. The nature of the products formed depends on the conditions used and the type of alkyne reacted. Reactions between I and terminal alkynes in the presence of ammonium hexafluorophosphate lead to the formation of cationic monosubstituted ruthenium vinylidene complexes in high yield, as shown for phenylacetylene in Eq. (61) (4,67,68). 

The tetrachloronickel(II) salt of the ligand cation is readily converted to the hexafluorophosphate salt. This procedure is necessary to avoid the reinsertion of any nickel(II) into the macrocyclic ligand during the neutralization process. Ten grams of [C22H26N4] [NiCl4] is dissolved in a minimum amount (about 100 mL) of water, and 9.0 g (1.5 excess) of ammonium hexafluorophosphate, also dissolved in a minimum amount (about 8 mL) of water, is added slowly. A colorless precipitate of the hexafluorophosphate salt [C22H26N4] [PF6]2 forms immediately. The product is filtered, washed with water, and air dried. The yield is quantitative. 

Cyclic voltammograms of C60F46 in a CH2CI2/O.I M TBAPF6 (tetrabutyl-ammonium hexafluorophosphate) solution are shown in Fig. 20 [33], The reduction of C60F46 to its anion radical occurs at the first half wave potential "1/2 = 0.51... 

Reaction of cobalt(III) acetate and ammonium hexafluorophosphate in methanol over one week at room temperature yielded a mixture of products that included green crystals of [NH,][Co (MeC02) (OMe),J[PF,]. The cavity in this product... 

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