Vernier-templated synthesis, crystal structure, and supramolecular chemistry of a 12-Porphyrin nanoring

Vernier templating exploits a mismatch between the number of binding sites in a template and a reactant to direct the formation of a product that is large enough to bind several template units. Here, we present a detailed study of the Vernier-templated synthesis of a 12-porphyrin nanoring. NMR and s...

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Main Authors: Kondratuk, Dmitry V., Sprafke, Johannes K., O'Sullivan, Melanie C., Perdigão, Luis M.A., Saywell, Alexander, Malfois, Marc, O'Shea, James N., Beton, Peter H., Thompson, Amber L., Anderson, Harry L.
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Published: Wiley-VCH Verlag 2014
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Online Access:https://eprints.nottingham.ac.uk/34935/
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author Kondratuk, Dmitry V.
Sprafke, Johannes K.
O'Sullivan, Melanie C.
Perdigão, Luis M.A.
Saywell, Alexander
Malfois, Marc
O'Shea, James N.
Beton, Peter H.
Thompson, Amber L.
Anderson, Harry L.
author_facet Kondratuk, Dmitry V.
Sprafke, Johannes K.
O'Sullivan, Melanie C.
Perdigão, Luis M.A.
Saywell, Alexander
Malfois, Marc
O'Shea, James N.
Beton, Peter H.
Thompson, Amber L.
Anderson, Harry L.
author_sort Kondratuk, Dmitry V.
building Nottingham Research Data Repository
collection Online Access
description Vernier templating exploits a mismatch between the number of binding sites in a template and a reactant to direct the formation of a product that is large enough to bind several template units. Here, we present a detailed study of the Vernier-templated synthesis of a 12-porphyrin nanoring. NMR and small-angle X-ray scattering (SAXS) analyses show that Vernier complexes are formed as intermediates in the cyclo-oligomerization reaction. UV/Vis/NIR titrations show that the three-component assembly of the 12-porphyrin nanoring figure-of-eight template complex displays high allosteric cooperativity and chelate cooperativity. This nanoring–template 1:2 complex is among the largest synthetic molecules to have been characterized by single-crystal analysis. It crystallizes as a racemate, with an angle of 27° between the planes of the two template units. The crystal structure reveals many unexpected intramolecular C[BOND]H⋅⋅⋅N contacts involving the tert-butyl side chains. Scanning tunneling microscopy (STM) experiments show that molecules of the 12-porphyrin template complex can remain intact on the gold surface, although the majority of the material unfolds into the free nanoring during electrospray deposition.
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spelling nottingham-349352020-05-04T16:52:07Z https://eprints.nottingham.ac.uk/34935/ Vernier-templated synthesis, crystal structure, and supramolecular chemistry of a 12-Porphyrin nanoring Kondratuk, Dmitry V. Sprafke, Johannes K. O'Sullivan, Melanie C. Perdigão, Luis M.A. Saywell, Alexander Malfois, Marc O'Shea, James N. Beton, Peter H. Thompson, Amber L. Anderson, Harry L. Vernier templating exploits a mismatch between the number of binding sites in a template and a reactant to direct the formation of a product that is large enough to bind several template units. Here, we present a detailed study of the Vernier-templated synthesis of a 12-porphyrin nanoring. NMR and small-angle X-ray scattering (SAXS) analyses show that Vernier complexes are formed as intermediates in the cyclo-oligomerization reaction. UV/Vis/NIR titrations show that the three-component assembly of the 12-porphyrin nanoring figure-of-eight template complex displays high allosteric cooperativity and chelate cooperativity. This nanoring–template 1:2 complex is among the largest synthetic molecules to have been characterized by single-crystal analysis. It crystallizes as a racemate, with an angle of 27° between the planes of the two template units. The crystal structure reveals many unexpected intramolecular C[BOND]H⋅⋅⋅N contacts involving the tert-butyl side chains. Scanning tunneling microscopy (STM) experiments show that molecules of the 12-porphyrin template complex can remain intact on the gold surface, although the majority of the material unfolds into the free nanoring during electrospray deposition. Wiley-VCH Verlag 2014-08-25 Article PeerReviewed Kondratuk, Dmitry V., Sprafke, Johannes K., O'Sullivan, Melanie C., Perdigão, Luis M.A., Saywell, Alexander, Malfois, Marc, O'Shea, James N., Beton, Peter H., Thompson, Amber L. and Anderson, Harry L. (2014) Vernier-templated synthesis, crystal structure, and supramolecular chemistry of a 12-Porphyrin nanoring. Chemistry - a European Journal, 20 . pp. 12826-12834. ISSN 1521-3765 Conjugation Macrocycles Porphyrinoids Supramolecular chemistry Template synthesis http://dx.doi.org/10.1002/chem.201403714 doi:10.1002/chem.201403714 doi:10.1002/chem.201403714
spellingShingle Conjugation
Macrocycles
Porphyrinoids
Supramolecular chemistry
Template synthesis
Kondratuk, Dmitry V.
Sprafke, Johannes K.
O'Sullivan, Melanie C.
Perdigão, Luis M.A.
Saywell, Alexander
Malfois, Marc
O'Shea, James N.
Beton, Peter H.
Thompson, Amber L.
Anderson, Harry L.
Vernier-templated synthesis, crystal structure, and supramolecular chemistry of a 12-Porphyrin nanoring
title Vernier-templated synthesis, crystal structure, and supramolecular chemistry of a 12-Porphyrin nanoring
title_full Vernier-templated synthesis, crystal structure, and supramolecular chemistry of a 12-Porphyrin nanoring
title_fullStr Vernier-templated synthesis, crystal structure, and supramolecular chemistry of a 12-Porphyrin nanoring
title_full_unstemmed Vernier-templated synthesis, crystal structure, and supramolecular chemistry of a 12-Porphyrin nanoring
title_short Vernier-templated synthesis, crystal structure, and supramolecular chemistry of a 12-Porphyrin nanoring
title_sort vernier-templated synthesis, crystal structure, and supramolecular chemistry of a 12-porphyrin nanoring
topic Conjugation
Macrocycles
Porphyrinoids
Supramolecular chemistry
Template synthesis
url https://eprints.nottingham.ac.uk/34935/
https://eprints.nottingham.ac.uk/34935/
https://eprints.nottingham.ac.uk/34935/