Synthesis and Characterization of the Monomeric Phosphinogallanes But2GaPR'R'' (R', R'' = bulky aryl or silyl groups) and Related Compounds

DOI: 10.1039/DT9930001737

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 1737 - 1746 (1993)

Update date:2022-08-04

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Authors:

Petrie, Mark A.

Power, Philip P.

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Article abstract of DOI:10.1039/DT9930001737

The use of bulky substituent groups has allowed the isolation and spectroscopic and structural characterization of several monomeric phosphinogallanes wherein gallium and phosphorus are three-co-ordinate.These new compounds have the formula Bu^t2GaP(R)(SiPh3) (R = C6H2Bu^t3-2,4,6 1, C6H2Prⁱ3-2,4,6 2, C6H2Me3-2,4,6 3 or SiMe3 4).Variable-temperature 1H NMR studies indicate that there is a rotational barrier of ca. 12.7 kcal mol^-1 around the Ga-P bond in 1 which has been attributed to weak Ga-P ? bonding.The synthesis and structures of the related aluminium-phosphorus species Bu^t2Al(Et2O)P(C6H2Prⁱ3-2,4,6)(SiPh3) 5 and the gallium-arsenic species Bu^t2GaAs(SiPh3) 6 are also reported.In addition, variable-temperature 1H NMR studies of the precursor asymmetric phosphines (Ph3Si)P(R)H (R =C6H2Bu^t3-2,4,6 7, C6H2Prⁱ2,4,6 8 or C6H2Me3-2,4,6 9) as well as the X-ray structures of (Ph3Si)P(C6H2Bu^t3-2,4,6)H 7 and (Ph3Si)P(SiMe3)2 10 are discussed.Crystal data with Mo-K_α radiation (λ = 0.71069 Angstroem) at 130 K: 2, monoclinic, space group P2₁/c, a = 18.499(5), b = 10.028(4), c = 20.746(6) Angstroem, β = 90.45(1) deg, Z = 4, R = 0.043; 5, triclinic, space group P<*>, a = 9.488(3), b = 11.416(5), c = 20.383(6) Angstroem, α = 92.07(3), β = 96.80(2), γ = 103.17(39 deg, Z = 2, R = 0.079; 6, triclinic, space group P<*>, a = 12.219(3), b = 14.174(3), c = 21.831(5) Angstroem, α = 92.95(2), β = 99.73(2), γ = 99.47(2) deg, Z =4, R = 0.053; 7, monoclinic, space group P2₁/c, a = 17.710(6), b = 16.635(5), c = 10.838(4) Angstroem, β = 97.43(3) deg, Z = 4, R = 0.044; 10, orthorhombic, space group Pbca, a = 16.092(5), b = 16.841(5), c = 18.778(5) Angstroem, Z = 8 and R = 0.050.

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