H. Mack et al., THERMAL-DECOMPOSITION OF [ME3SINCH2CH2NSIME3]CENTER-DOT-LI-2(THF)(2) TO [LIN(SIME3)(2)CENTER-DOT-THF](2) VIA A 1,4-TRIMETHYLSILYL SHIFT, Journal of organometallic chemistry, 549(1-2), 1997, pp. 39-43
The dilithium salt [Me3SiNCH2CH2NSiMe3].Li-2(THF)(2) decomposes slowly
upon heating forming a metastable structure of the crystalline [LiN(S
iMe3).THF](2). The crystal structure of the new form was established b
y single crystal X-ray diffraction showing a decrease in the a and b p
arameter values of the unit cell, and an expansion of the c value as c
ompared with the structure obtained at room temperature. The major dis
crepancies among the known and the metastable crystalline framework ar
e the Li-O bond length and the dihedral angle disposition of the trime
thylsilyl groups as regarded to the middle Li-N-Li-N heterocyclobutane
ring. Attempts to trap the expected additional lithium imine product
were unsuccessful although quenching experiments produced polyethylene
imine. (C) 1997 Elsevier Science S.A.