Synthesis and Characterization of the Monomeric Gallium Monoamides t-Bu2GaN(R)SiPh3 (R = t-Bu, 1-Adamantyl), Trip2MN(H)Dipp (M = Al, Ga; Trip = 2,4,6-i-Pr3C6H2; Dipp = 2,6-i-Pr2C6H3), and Trip2GaNPh2

K. M. Waggoner, K. Ruhlandt-Senge, R. J. Wehmschulte, X. He, M. M. Olmstead, P. P. Power

Research output: Contribution to journalArticle

61 Scopus citations

Abstract

The synthesis and characterization of the monomeric, main group 3 monoamides t-Bu2GaN(R)(SiPh3) (R = t-Bu (1); R = 1-Adamantyl (1-Ad) (2)), Trip2MN(H)Dipp (M = Al (3); M = Ga (4)) (Trip = 2,4,6-i-Pr3C6H2, Dipp = 2,6-i-Pr2C6H3), and Trip2GaNPh2 (5) are described. The compounds were characterized by X-ray crystallography and 1H NMR and IR spectroscopy. The crystal structures show the molecules to be monomeric with trigonal planar metal and nitrogen coordination. The Ga-N bond lengths range from 1.847(12) Å in 4 to 1.924(2) Å in 2. The Al-N bond length observed in 3 is 1.784(3) Å. The variation may be explained mostly on the basis of different steric and electronic properties of the bulky ligands. It was concluded, on the basis of VT 1H NMR data, that the p-p π-bonding contribution to M-Nbond strength in the aluminum or gallium species is <10 kcal mol−1. Crystal data at 130 K, with Mo Kα (λ = 0.71069 Å) radiation, are as follows: t-Bu2GaN(t-Bu)SiPh3 (1), a = 14.795(6) Å, b = 9.807(6) Å, c = 19.657(9) Å, β = 99.39(4)°, V = 2824(1) Å3, space group P21/c, Z = 4, 2361 (I > 2σ(I)) data, R = 0.053; t-Bu2GaN(l-Ad)SiPh3 (2), a = 10.191(3) Å, b = 10.740(3) Å, c = 15.467(5) Å, α = 69.82(2)°, β = 82.79(2)°, γ = 82.75(2)°, V = 1568.4(8) Å3, space group P1̅, Z = 2, 5130 (I > 3σ (I)) data, R = 0.037; Trip2AlN(H)Dipp (3), a = 11.643(5) Å, b = 18.460(6) Å, c = 37.165(14) Å, β = 95.86(3)°, V= 7947(5) Å3, space group C2/c, Z = 8, 3639 (I > 2σ(I)) data, R = 0.056; Trip2GaN(H)Dipp (4), a = 11.588(8) Å, b = 18.496(14) Å, c = 37.27(2) Å,β = 95.17°, V = 7956(9) Å3, space group C2/c, Z = 8, 1837 (I > 2σ(I)) data, R = 0.084; Trip2GaNPh2 (5), a = 12.732(4) Å, b = 15.656(5) Å, c = 18.462(6) Å, V = 3680(2) Å3, space group Pccn, Z = 4, 1944 (I > 2σ(I)) data, R = 0.092.

Original languageEnglish (US)
Pages (from-to)2557-2561
Number of pages5
JournalInorganic Chemistry
Volume32
Issue number11
DOIs
StatePublished - Jan 1 1993
Externally publishedYes

ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry

Fingerprint Dive into the research topics of 'Synthesis and Characterization of the Monomeric Gallium Monoamides t-Bu<sub>2</sub>GaN(R)SiPh<sub>3</sub> (R = t-Bu, 1-Adamantyl), Trip<sub>2</sub>MN(H)Dipp (M = Al, Ga; Trip = 2,4,6-i-Pr<sub>3</sub>C<sub>6</sub>H<sub>2</sub>; Dipp = 2,6-i-Pr<sub>2</sub>C<sub>6</sub>H<sub>3</sub>), and Trip<sub>2</sub>GaNPh<sub>2</sub>'. Together they form a unique fingerprint.

  • Cite this