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, Karin Ruhlandt, R. J. Wehmschulte, X. He, M. M. Olmstead, P. P. Power

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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(1-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 P1, 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
StatePublished - 1993
Externally publishedYes

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Gallium
Bond length
gallium
X ray crystallography
synthesis
Aluminum
Electronic properties
Nuclear magnetic resonance spectroscopy
Infrared spectroscopy
Nitrogen
Crystal structure
Metals
Nuclear magnetic resonance
Ligands
Molecules
nuclear magnetic resonance
crystallography
aluminum
nitrogen
ligands

ASJC Scopus subject areas

  • Inorganic Chemistry

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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 . / Waggoner, K. M.; Ruhlandt, Karin; Wehmschulte, R. J.; He, X.; Olmstead, M. M.; Power, P. P.

In: Inorganic Chemistry, Vol. 32, No. 11, 1993, p. 2557-2561.

Research output: Contribution to journalArticle

@article{819f8da1a8d94219ae3edba8aa32267b,
title = "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",
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) {\AA} in 4 to 1.924(2) {\AA} in 2. The Al-N bond length observed in 3 is 1.784(3) {\AA}. 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 {\AA}) radiation, are as follows: t-Bu2GaN(t-Bu)SiPh3 (1), a = 14.795(6) {\AA}, b = 9.807(6) {\AA}, c = 19.657(9) {\AA}, β = 99.39(4)°, V = 2824(1) {\AA}3, space group P21/c, Z = 4, 2361 (I > 2σ(I)) data, R = 0.053; t-Bu2GaN(1-Ad)SiPh3 (2), a = 10.191(3) {\AA}, b = 10.740(3) {\AA}, c = 15.467(5) {\AA}, α = 69.82(2)°, β = 82.79(2)°, γ = 82.75(2)°, V = 1568.4(8) {\AA}3, space group P1, Z = 2, 5130 (I > 3σ (I)) data, R = 0.037; Trip2AlN(H)Dipp (3), a = 11.643(5) {\AA}, b = 18.460(6) {\AA}, c = 37.165(14) {\AA}, β = 95.86(3)°, V = 7947(5) {\AA}3, space group C2/c, Z = 8, 3639 (I > 2σ(I)) data, R = 0.056; Trip2GaN(H)Dipp (4), a = 11.588(8) {\AA}, b = 18.496(14) {\AA}, c = 37.27(2) {\AA}, β = 95.17°, V = 7956(9) {\AA}3, space group C2/c, Z = 8, 1837 (I > 2σ(I)) data, R = 0.084; Trip2GaNPh2 (5), a = 12.732(4) {\AA}, b = 15.656(5) {\AA}, c = 18.462(6) {\AA}, V = 3680(2) {\AA}3, space group Pccn, Z = 4, 1944 (I > 2σ(I)) data, R = 0.092.",
author = "Waggoner, {K. M.} and Karin Ruhlandt and Wehmschulte, {R. J.} and X. He and Olmstead, {M. M.} and Power, {P. P.}",
year = "1993",
language = "English (US)",
volume = "32",
pages = "2557--2561",
journal = "Inorganic Chemistry",
issn = "0020-1669",
publisher = "American Chemical Society",
number = "11",

}

TY - JOUR

T1 - 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

AU - Waggoner, K. M.

AU - Ruhlandt, Karin

AU - Wehmschulte, R. J.

AU - He, X.

AU - Olmstead, M. M.

AU - Power, P. P.

PY - 1993

Y1 - 1993

N2 - 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(1-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 P1, 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.

AB - 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(1-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 P1, 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.

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