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

doi:10.1021/ic00112a033

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

Chemistry (Twin Cities)

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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 language	English (US)
Pages (from-to)	2179-2185
Number of pages	7
Journal	Inorganic chemistry
Volume	34
Issue number	8
DOIs	https://doi.org/10.1021/ic00112a033
State	Published - Apr 1 1995

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@article{82fd35e984034b5eb238e03ac4f5c192,

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

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) {\AA}, b = 9.579(2) {\AA}, c = 19.881(2) {\AA}, α = 94.98(1)°, β = 93.27(1)°, γ = 103.51(1)°, V = 1692.4(4) {\AA}3, Z = 2, space group P1, R = 0.0592; 3, trigonal with a = 12.449(1) {\AA},b = 12.449(1) {\AA}, c = 28.251(6) {\AA}, V= 3791.7(9) {\AA}3, 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.",

author = "Zhibang Duan and Young, {Victor G.} and Verkade, {John G.}",

year = "1995",

month = apr,

day = "1",

doi = "10.1021/ic00112a033",

language = "English (US)",

volume = "34",

pages = "2179--2185",

journal = "Inorganic Chemistry",

issn = "0020-1669",

publisher = "American Chemical Society",

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TY - JOUR

T1 - Syntheses and Structures of Lithiated Tetramines

T2 - [Li3(Me3SiNCH2CH2)3N(THF)2] and {(μ3-Cl)Li3H4[(Me3SiNCH2CH2)3N]2}

AU - Duan, Zhibang

AU - Young, Victor G.

AU - Verkade, John G.

PY - 1995/4/1

Y1 - 1995/4/1

N2 - 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.

AB - 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.

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U2 - 10.1021/ic00112a033

DO - 10.1021/ic00112a033

M3 - Article

AN - SCOPUS:0000472777

SN - 0020-1669

VL - 34

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JO - Inorganic Chemistry

JF - Inorganic Chemistry

IS - 8

ER -

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

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