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Metallaheteroborane Chemistry. Part 12. Synthesis of Cationic Metallaheteroboranes ; Molecular Structures of the Compounds with L = H2O or CO

DOI: 10.1039/DT9930000035

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 35 - 42 (1993)

Update date:2022-08-04

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Authors:

Sheehan, James P.Sheehan, James P.

Spalding, Trevor R.Spalding, Trevor R.

Ferguson, GeorgeFerguson, George

Gallagher, John F.Gallagher, John F.

Kaitner, BrankoKaitner, Branko

Kennedy, John D.Kennedy, John D.

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Article abstract of DOI:10.1039/DT9930000035

The reaction of Ag and <2-I-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)> 2 in excellent yield.This complex has been characterised by (IR and (11)B NMR) spectroscopy and X-ray crystallography.Crystals of 2*0.89CH2Cl2 are monoclinic, space group P21/c, with cell dimensions a = 14.073, b = 15.640(2), c = 20.262(6) Angstroem and β = 94.80(2) deg.A final R factor of 0.038 was claculated for 5595 observed reflections.The Pd-OH2 distance is 2.208(4) Angstroem and Pd-P(1) is 2.3544(14) Angstroem.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) Angstroem.The exo-cage B(7)-P(2) distance is 1.950(6) Angstroem.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)> t, CNC6H11, NCMe, MeCH(Ph)NH2, OC4H8 or SC4H8> in yields ranging from 39 to 93percent.Reaction between 2 and a tenfold excess of PMe2Ph affords <2,2-(PMe2Ph)2-closo-2,1-PdTeB10H9(PPh3)> in 75percent yield.All complexes have been characterised spectroscopically (IR and (11)B NMR) and in the case of <2-(CO)-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)> 3 by X-ray crystallography.The 3*C6H5Me solvate crystallises in the monoclinic spce group P21/c with Z = 4, a = 14.509(3), b = 10.732(1), c = 31.377(8) Angstroem and β = 97.49(2) deg.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) Angstroem.

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Product name:{2-(CO)-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)}{BF4} * C6H5Me

Cas No:147133-79-7

147133-79-7

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