147104-97-0Relevant academic research and scientific papers
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)
Ferguson, George,Gallagher, John F.,McGrath, Marguerite,Sheehan, James P.,Spalding, Trevor R.,Kennedy, John D.
, p. 27 - 34 (1993)
Reaction of (R3 = Ph3, MePh2 or Me2Ph) with the nido-(1-) anions (E = Se or Te) in tetrahydrofuran (thf) at ambient temperature affords twelve-vertex 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 (1-) in refluxing toluene affords only in 39 and 95percent yields respectively.Further reactions of with HgII salts in thf produce 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- NMR spectroscopy of shows a metal-to-selenaborane rotational bonding fluxionality with ΔG(excit.)293 = 44.5 kJ mol-1.An X-ray diffraction study of 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 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,
