Issue 1, 1993

Metallaheteroborane chemistry. Part 12. Synthesis of cationic metallaheteroboranes [2-L-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)][BF4]; molecular structures of the compounds with L = H2O or CO

Abstract

The reaction of Ag[BF4] and [2-l-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)]1 in toluene for 30 min at room temperature and subsequent isolation of the product under aerobic conditions afforded [2-(H2O)-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)][BF4]2 in excellent yield. This complex has been characterised by (IR and 11B NMR) spectroscopy and X-ray crystallography. Crystals of 2·0.89CH2Cl2 are monoclinic, space group P21/c, with cell dimensions a= 14.073(3), b= 15.640(2), c= 20.262(6)Å and β= 94.80(2)°. A final R factor of 0.038 was calculated for 5595 observed reflections. The Pd–OH2 distance is 2.208(4)Å and Pd–P(1) is 2.3544(14)Å. Cage interatomic distances include Pd–Te 2.6958(6) and ranges for Pd–B of 2.192(6)–2.299(6) and Te–B of 2.287(6)–2.403(6)Å. The exo-cage B(7)–P(2) distance is 1.950(6)Å. The water molecule in 2 can be displaced by a variety of ligands to produce the cationic palladatelluraborane complexes [2-L-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)][BF4][L = CO, CNBut, CNC6H11, NCMe, MeCH(Ph)NH2, OC4H8 or SC4H8) in yields ranging from 39 to 93%. Reaction between 2 and a ten-fold excess of PMe2Ph affords [2,2-(PMe2Ph)2-closo-2,1-PdTeB10H9(PPh3)][BF4] in 75% yield. All complexes have been characterised spectroscopically (IR and 11B NMR) and in the case of [2-(CO)-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)][BF4]3 by X-ray crystallography. The 3·C6H5Me solvate crystallises in the monoclinic space group P21/c with Z= 4, a= 14.509(3), b= 10.732(1), c= 31.377(8)Å and β= 97.49(2)°. The final R factor of 0.054 was calculated from 5439 observed reflections. Principal interatomic distances include Pd–Te 2.6897(9), Pd–B 2.195(10)–2.307(9), Te–B 2.262(11)–2.389(9), Pd–P(2) 2.367(2), B(11)–P(1) 1.941(9) and Pd–C(1) 2.003(9)Å.

Article information

Article type
Paper

J. Chem. Soc., Dalton Trans., 1993, 35-42

Metallaheteroborane chemistry. Part 12. Synthesis of cationic metallaheteroboranes [2-L-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)][BF4]; molecular structures of the compounds with L = H2O or CO

J. P. Sheehan, T. R. Spalding, G. Ferguson, J. F. Gallagher, B. Kaitner and J. D. Kennedy, J. Chem. Soc., Dalton Trans., 1993, 35 DOI: 10.1039/DT9930000035

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