Chemically cross-linked polyacrylonitrile. A DMSO compatible NMR alignment medium for measurement of residual dipolar couplings and residual chemical shift anisotropies

Daiane S Carvalho; Danilo G B da Silva; Fernando Hallwass; Armando Navarro-Vázquez

doi:10.1016/j.jmr.2019.03.005

Chemically cross-linked polyacrylonitrile. A DMSO compatible NMR alignment medium for measurement of residual dipolar couplings and residual chemical shift anisotropies

J Magn Reson. 2019 May:302:21-27. doi: 10.1016/j.jmr.2019.03.005. Epub 2019 Mar 15.

Authors

Daiane S Carvalho¹, Danilo G B da Silva¹, Fernando Hallwass¹, Armando Navarro-Vázquez²

Affiliations

¹ Universidade Federal de Pernambuco, Departamento de Química Fundamental, CCEN, Recife, Pernambuco 50670-901, Brazil.
² Universidade Federal de Pernambuco, Departamento de Química Fundamental, CCEN, Recife, Pernambuco 50670-901, Brazil. Electronic address: [email protected].

PMID: 30933840
DOI: 10.1016/j.jmr.2019.03.005

Abstract

Chemically cross-linked polyacrylontrile polymer gels, have been prepared as an alignment medium compatible with DMSO-d₆. These gels allow measurement of residual dipolar couplings (RDCs) and residual chemical shift anisotropies (RCSAs) with good accuracy as tested with brucine and α-santonin natural compounds. The gels can be reversibly compressed allowing easy measurement of RCSAs. They also present good physical homogeneity, clean HSQC spectra with little background ¹H signals, and allow unambiguous referencing of ¹³C spectra for RCSA extraction.

Keywords: Alignment media; Natural products; RCSAs; RDCs; Stereochemistry; Structural elucidation.

Publication types

Research Support, Non-U.S. Gov't