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
SP - 2179
EP - 2185
JO - Inorganic chemistry
JF - Inorganic chemistry
IS - 8
ER -