Syntheses and Structures of Lithiated Tetramines: [Li3(Me3SiNCH2CH2)3N(THF)2] and {(μ3-Cl)Li3H4[(Me3SiNCH2CH2)3N]2}

Zhibang Duan, Victor G. Young, John G. Verkade

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Abstract

The compounds [Li3(Me3SiNCH2CH2)3N(THF)2], 2, and {(μ3-Cl)Li3H4[(Me3SiNCH2CH2)3N]2},3, were synthesized and characterized by 13C, 29Si, and 7Li NMR spectroscopies, and their structures were determined by single crystal X-ray crystallography. Compound 2 was shown to contain a trigonal monopyramidal lithium center while 3 utilizes a LiCl to link two amido triamine ligands together. Crystal data: 2, triclinic with a = 9.2035(8) Å, b = 9.579(2) Å, c = 19.881(2) Å, α = 94.98(1)°, β = 93.27(1)°, γ = 103.51(1)°, V = 1692.4(4) Å3, Z = 2, space group P1, R = 0.0592; 3, trigonal with a = 12.449(1) Å,b = 12.449(1) Å, c = 28.251(6) Å, V= 3791.7(9) Å3, Z = 3, space group P32, 50:50 y, x, z twin, R = 0.0249. Variable-temperature 1H and 7Li NMR spectral studies reveal a dynamic behavior of 2 in solution. WH DQF COSY, 1H13C-heterocorrelated 2D, and VT NMR experiments confirm that the structure of 3 in solution is the same as that in the solid state.

Original languageEnglish (US)
Pages (from-to)2179-2185
Number of pages7
JournalInorganic chemistry
Volume34
Issue number8
DOIs
StatePublished - Apr 1 1995

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