Synthesis of Li(I), Zn(II) and Mg(II) complexes of amine bis(phenolates) and their exploitation for the ring opening polymerisation of rac-lactide

Helena Quilter, Rachel Drewitt, Mary Mahon, Gabriele Kociok-Kohn, Matthew Jones

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Abstract

In this paper a series of Mg(II), Li(I) and Zn(II) complexes based on two families of amine bis(phenolate)s have been prepared and structurally characterised. In the solid-state the Li(I) complexes form common Li4O4 cubes and there are subtle differences in coordination mode between the two salan ligands employed. We also have prepared a Li3Mg1O4 cube structure, by the reaction of 1 eq. of ligand 2H2, with 1 eq. of both nBuLi and MgnBu2. Upon addition of the ligands with Zn(II) either a trimetallic or tetrametallic structure was isolated. With 2H2 a complex with an –OMe was observed, this arises from the insertion of oxygen into the Zn-Me bond. Upon reaction with MgnBu2 dimeric complexes were isolated. All complexes were tested for the ROP of rac-lactide in solution. High molecular weight polylactide was isolated with narrow molecular weight distributions being observed. In most cases PLA with a very slight heterotactic bias was formed.
LanguageEnglish
Pages325-331
JournalJournal of Organometallic Chemistry
Volume848
Early online date24 Aug 2017
DOIs
StatusPublished - 15 Oct 2017

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Ring opening polymerization
exploitation
Polymerization
Amines
amines
polymerization
Ligands
ligands
rings
molecular weight
synthesis
Molecular Weight
Molecular weight distribution
insertion
Molecular weight
Oxygen
solid state
oxygen
dilactide

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Synthesis of Li(I), Zn(II) and Mg(II) complexes of amine bis(phenolates) and their exploitation for the ring opening polymerisation of rac-lactide. / Quilter, Helena; Drewitt, Rachel; Mahon, Mary; Kociok-Kohn, Gabriele; Jones, Matthew.

In: Journal of Organometallic Chemistry, Vol. 848, 15.10.2017, p. 325-331.

Research output: Contribution to journal › Article

Quilter, H, Drewitt, R, Mahon, M, Kociok-Kohn, G & Jones, M 2017, 'Synthesis of Li(I), Zn(II) and Mg(II) complexes of amine bis(phenolates) and their exploitation for the ring opening polymerisation of rac-lactide' Journal of Organometallic Chemistry, vol. 848, pp. 325-331. DOI: 10.1016/j.jorganchem.2017.08.014
Quilter H, Drewitt R, Mahon M, Kociok-Kohn G, Jones M. Synthesis of Li(I), Zn(II) and Mg(II) complexes of amine bis(phenolates) and their exploitation for the ring opening polymerisation of rac-lactide. Journal of Organometallic Chemistry. 2017 Oct 15;848:325-331. Available from, DOI: 10.1016/j.jorganchem.2017.08.014
Quilter, Helena ; Drewitt, Rachel ; Mahon, Mary ; Kociok-Kohn, Gabriele ; Jones, Matthew. / Synthesis of Li(I), Zn(II) and Mg(II) complexes of amine bis(phenolates) and their exploitation for the ring opening polymerisation of rac-lactide. In: Journal of Organometallic Chemistry. 2017 ; Vol. 848. pp. 325-331
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abstract = "In this paper a series of Mg(II), Li(I) and Zn(II) complexes based on two families of amine bis(phenolate)s have been prepared and structurally characterised. In the solid-state the Li(I) complexes form common Li4O4 cubes and there are subtle differences in coordination mode between the two salan ligands employed. We also have prepared a Li3Mg1O4 cube structure, by the reaction of 1 eq. of ligand 2H2, with 1 eq. of both nBuLi and MgnBu2. Upon addition of the ligands with Zn(II) either a trimetallic or tetrametallic structure was isolated. With 2H2 a complex with an –OMe was observed, this arises from the insertion of oxygen into the Zn-Me bond. Upon reaction with MgnBu2 dimeric complexes were isolated. All complexes were tested for the ROP of rac-lactide in solution. High molecular weight polylactide was isolated with narrow molecular weight distributions being observed. In most cases PLA with a very slight heterotactic bias was formed.",
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N2 - In this paper a series of Mg(II), Li(I) and Zn(II) complexes based on two families of amine bis(phenolate)s have been prepared and structurally characterised. In the solid-state the Li(I) complexes form common Li4O4 cubes and there are subtle differences in coordination mode between the two salan ligands employed. We also have prepared a Li3Mg1O4 cube structure, by the reaction of 1 eq. of ligand 2H2, with 1 eq. of both nBuLi and MgnBu2. Upon addition of the ligands with Zn(II) either a trimetallic or tetrametallic structure was isolated. With 2H2 a complex with an –OMe was observed, this arises from the insertion of oxygen into the Zn-Me bond. Upon reaction with MgnBu2 dimeric complexes were isolated. All complexes were tested for the ROP of rac-lactide in solution. High molecular weight polylactide was isolated with narrow molecular weight distributions being observed. In most cases PLA with a very slight heterotactic bias was formed.

AB - In this paper a series of Mg(II), Li(I) and Zn(II) complexes based on two families of amine bis(phenolate)s have been prepared and structurally characterised. In the solid-state the Li(I) complexes form common Li4O4 cubes and there are subtle differences in coordination mode between the two salan ligands employed. We also have prepared a Li3Mg1O4 cube structure, by the reaction of 1 eq. of ligand 2H2, with 1 eq. of both nBuLi and MgnBu2. Upon addition of the ligands with Zn(II) either a trimetallic or tetrametallic structure was isolated. With 2H2 a complex with an –OMe was observed, this arises from the insertion of oxygen into the Zn-Me bond. Upon reaction with MgnBu2 dimeric complexes were isolated. All complexes were tested for the ROP of rac-lactide in solution. High molecular weight polylactide was isolated with narrow molecular weight distributions being observed. In most cases PLA with a very slight heterotactic bias was formed.

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