Novel Ti(IV) and Zr(IV) complexes and their application in the ring-opening polymerisation of cyclic esters

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Abstract

A series of group 4 amine tris(phenolate) complexes have been prepared and characterised by single crystal X-ray diffraction and multinuclear NMR spectroscopy. It was found that the ligands afforded monomeric titanium complexes and dimeric zirconium structures in the solid-state. The complexes have been tested for the ring-opening polymerisation of rac-lactide under both solution and melt conditions, which showed varying degrees of selectivity and control, with PDIs in the range of 1.09-2.07. The initiators were also tested for the production of copolymers containing rac-lactide and isosorbide. From NMR spectroscopic analysis and MALDI-TOF mass spectrometry the isosorbide is incorporated into the polymer. The complexes were also screened for the ring-opening polymerisation of 1,3-dioxan-2-one to produce a polycarbonate with good conversions (24-99%).
Original languageEnglish
Pages (from-to)9020-9025
Number of pages6
JournalDalton Transactions
Volume41
DOIs
Publication statusPublished - 2009

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Isosorbide
polycarbonate
Ring opening polymerization
Esters
Spectroscopic analysis
Titanium
Nuclear magnetic resonance spectroscopy
Amines
Mass spectrometry
Polymers
Copolymers
Nuclear magnetic resonance
Single crystals
Ligands
X ray diffraction
dilactide
1,4-dioxane

Cite this

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title = "Novel Ti(IV) and Zr(IV) complexes and their application in the ring-opening polymerisation of cyclic esters",
abstract = "A series of group 4 amine tris(phenolate) complexes have been prepared and characterised by single crystal X-ray diffraction and multinuclear NMR spectroscopy. It was found that the ligands afforded monomeric titanium complexes and dimeric zirconium structures in the solid-state. The complexes have been tested for the ring-opening polymerisation of rac-lactide under both solution and melt conditions, which showed varying degrees of selectivity and control, with PDIs in the range of 1.09-2.07. The initiators were also tested for the production of copolymers containing rac-lactide and isosorbide. From NMR spectroscopic analysis and MALDI-TOF mass spectrometry the isosorbide is incorporated into the polymer. The complexes were also screened for the ring-opening polymerisation of 1,3-dioxan-2-one to produce a polycarbonate with good conversions (24-99{\%}).",
author = "Whitelaw, {E L} and Jones, {M D} and Mahon, {M F} and G Kociok-Kohn",
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T1 - Novel Ti(IV) and Zr(IV) complexes and their application in the ring-opening polymerisation of cyclic esters

AU - Whitelaw, E L

AU - Jones, M D

AU - Mahon, M F

AU - Kociok-Kohn, G

PY - 2009

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N2 - A series of group 4 amine tris(phenolate) complexes have been prepared and characterised by single crystal X-ray diffraction and multinuclear NMR spectroscopy. It was found that the ligands afforded monomeric titanium complexes and dimeric zirconium structures in the solid-state. The complexes have been tested for the ring-opening polymerisation of rac-lactide under both solution and melt conditions, which showed varying degrees of selectivity and control, with PDIs in the range of 1.09-2.07. The initiators were also tested for the production of copolymers containing rac-lactide and isosorbide. From NMR spectroscopic analysis and MALDI-TOF mass spectrometry the isosorbide is incorporated into the polymer. The complexes were also screened for the ring-opening polymerisation of 1,3-dioxan-2-one to produce a polycarbonate with good conversions (24-99%).

AB - A series of group 4 amine tris(phenolate) complexes have been prepared and characterised by single crystal X-ray diffraction and multinuclear NMR spectroscopy. It was found that the ligands afforded monomeric titanium complexes and dimeric zirconium structures in the solid-state. The complexes have been tested for the ring-opening polymerisation of rac-lactide under both solution and melt conditions, which showed varying degrees of selectivity and control, with PDIs in the range of 1.09-2.07. The initiators were also tested for the production of copolymers containing rac-lactide and isosorbide. From NMR spectroscopic analysis and MALDI-TOF mass spectrometry the isosorbide is incorporated into the polymer. The complexes were also screened for the ring-opening polymerisation of 1,3-dioxan-2-one to produce a polycarbonate with good conversions (24-99%).

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