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Metallaheteroborane Chemistry. Part 11. Selective Syntheses of the Palladium Heteroborane Complexes (R3 = Ph3, MePh2 or Me2Ph; E = Se or Te) and (X = Cl, Br, I, CN, SCN or O2CMe)

DOI: 10.1039/DT9930000027

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 27 - 34 (1993)

Update date:2022-08-05

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Authors:

Ferguson, GeorgeFerguson, George

Gallagher, John F.Gallagher, John F.

McGrath, MargueriteMcGrath, Marguerite

Sheehan, James P.Sheehan, James P.

Spalding, Trevor R.Spalding, Trevor R.

Kennedy, John D.Kennedy, John D.

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Article abstract of DOI:10.1039/DT9930000027

Reaction of (R3 = Ph3, MePh2 or Me2Ph) with the nido-<7-EB10H11>(1-) anions (E = Se or Te) in tetrahydrofuran (thf) at ambient temperature affords twelve-vertex <2,2-(PR3)2-closo-2,1-PdEB10H10> complexes selectively in yields ranging from 16 (E = Se, R = Ph) to 82percent (E = Te, R3 = Me3Ph).In contrast, the reaction between (X = Cl or I) and <7-TeB10H11>(1-) in refluxing toluene affords only <2-X-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)> in 39 and 95percent yields respectively.Further reactions of <2-I-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)> with HgII salts in thf produce <2-X-2-(PPh3)-closo-2,1-PdB10H9(PPh3)> complexes (X = Cl, Br, CN, SCN, or O2CMe) in yields from 19 (X = O2CMe) to 96percent (X = CN).All complexes were characterised by infrared and NMR spectroscopies.Variable-temperature (1)H-<(31)P> NMR spectroscopy of <2,2-(PMe2Ph)2-closo-2,1-PdSeB10H10> shows a metal-to-selenaborane rotational bonding fluxionality with ΔG(excit.)293 = 44.5 kJ mol-1.An X-ray diffraction study of <2,2-(PMe2Ph)2-closo-2,1-PdTeB10H10> 6 reveals the crystals to be monoclinic, space group P21/n, with a = 13.110(3), b = 10.498(3), c = 19.561(3) Angstroem, β = 105.44(1) deg and Z = 4.A final R factor of 0.023 was calculated for 4579 observed reflections.Principal interatomic distances include Pd-Te 2.6833(2), Pd-B 2.234(3)-2.301(3), Te-B 2.294(4)-2.374(3) and Pd-P 2.3301(7) and 2.3354(8) Angstroem.An X-ray diffraction study of <2-(O2CMe)-2-(PPh3)-closo-2,1-PdTeB10H9(PPh3)> 14 recrystallised from CH2Cl2-n-C7H14 as 14*0.79CH2Cl2 shows the crystals to be triclinic, space group P<*> with a = 10.416(2), b = 12.409(2), c = 18.720(4) Angstroem, α = 75.59(2), β = 84.10(2), γ = 70.98(1) deg and Z = 2.The final R factor is 0.035 for 6472 observed reflections.The acetate ligand is monodentate with Pd-O(1) 2.121(3) Angstroem.Other interatomic distances include Pd-Te 2.6903(49, Pd-P(2) 2.355(1), Pd-B(7) 2.201(5), Pd-B(6) 2.268(4) and B(11)-P(1) 1.942(4) Angstroem,

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