TY - JOUR
T1 - Synthesis and characterisation of magnesium complexes containing sterically demanding N,N′-bis(aryl)amidinate ligands
AU - Moxey, Graeme J.
AU - Ortu, Fabrizio
AU - Goldney Sidley, Leon
AU - Strandberg, Helen N.
AU - Blake, Alexander J.
AU - Lewis, William
AU - Kays, Deborah L.
PY - 2014/3/28
Y1 - 2014/3/28
N2 - Condensation reactions of carboxylic acids and anilines in the presence of polyphosphoric acid trimethylsilyl ester (PPSE) afforded a range of sterically demanding N,N′-bis(aryl)amidines, RN{C(R′)}N(H)R [R = Mes (Mes = 2,4,6-trimethylphenyl), R′ = Cy (Cy = cyclohexyl) L1H; R = Dipp (Dipp = 2,6-diisopropylphenyl), R′ = Cy L2H; R = Mes, R′ = Ph L3H; R = Dipp, R′ = Ph L4H; R = Mes, R′ = Dmp (Dmp = 3,5-dimethylphenyl) L5H; R = Dipp, R′ = Dmp L 6H; R = Dmp, R′ = Cy L7H]. Amidines L 1H-L7H have been characterised spectroscopically, and for L5H and L6H, by X-ray crystallography. Treatment of the amidines with di-n-butylmagnesium in THF solution afforded the monomeric magnesium bis(amidinates) [Mg(L1)2(THF)] 1, [Mg(L 2)2] 2, [Mg(L3)2(THF)] 3, [Mg(L 5)2(THF)] 5, [Mg(L6)2] 6, [Mg(L 7)2] 7, and the magnesium mono(amidinate) complex [Mg(L4)(nBu)] 4. These complexes have been characterised spectroscopically, with 1-3, 5 and 6 also being structurally authenticated. Comparison of the magnesium bis(amidinate) complexes reveals that the steric bulk of the amidinate ligand influences both the solid state structure and solution behaviour of these complexes.
AB - Condensation reactions of carboxylic acids and anilines in the presence of polyphosphoric acid trimethylsilyl ester (PPSE) afforded a range of sterically demanding N,N′-bis(aryl)amidines, RN{C(R′)}N(H)R [R = Mes (Mes = 2,4,6-trimethylphenyl), R′ = Cy (Cy = cyclohexyl) L1H; R = Dipp (Dipp = 2,6-diisopropylphenyl), R′ = Cy L2H; R = Mes, R′ = Ph L3H; R = Dipp, R′ = Ph L4H; R = Mes, R′ = Dmp (Dmp = 3,5-dimethylphenyl) L5H; R = Dipp, R′ = Dmp L 6H; R = Dmp, R′ = Cy L7H]. Amidines L 1H-L7H have been characterised spectroscopically, and for L5H and L6H, by X-ray crystallography. Treatment of the amidines with di-n-butylmagnesium in THF solution afforded the monomeric magnesium bis(amidinates) [Mg(L1)2(THF)] 1, [Mg(L 2)2] 2, [Mg(L3)2(THF)] 3, [Mg(L 5)2(THF)] 5, [Mg(L6)2] 6, [Mg(L 7)2] 7, and the magnesium mono(amidinate) complex [Mg(L4)(nBu)] 4. These complexes have been characterised spectroscopically, with 1-3, 5 and 6 also being structurally authenticated. Comparison of the magnesium bis(amidinate) complexes reveals that the steric bulk of the amidinate ligand influences both the solid state structure and solution behaviour of these complexes.
UR - http://www.scopus.com/inward/record.url?scp=84894836824&partnerID=8YFLogxK
U2 - 10.1039/c3dt53234h
DO - 10.1039/c3dt53234h
M3 - Article
SN - 1477-9226
VL - 43
SP - 4838
EP - 4846
JO - Dalton Transactions
JF - Dalton Transactions
IS - 12
ER -