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Rapid 3D NMR using the filter diagonalization method



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Journal of Magnetic Resonance 170 2004 156 163 www elsevier com locate jmr Rapid 3D NMR using the lter diagonalization method application to oligosaccharides derivatized with 13C labeled acetyl groups Geo rey S Armstrong a 1 Kristin E Cano a Vladimir A Mandelshtam a A J Shaka a and Brad Bendiakb b a Chemistry Department University of California Irvine CA 92697 2025 USA Department of Cell and Developmental Biology and Biomolecular Structure Program University of Colorado Health Sciences Center Box B111 4200 East Ninth Avenue Denver CO 80262 USA Received 7 April 2004 revised 4 June 2004 Available online 20 July 2004 Abstract Rapid 3D NMR spectroscopy of oligosaccharides having isotopically labeled acetyl isotags was made possible with high resolution in the indirect dimensions using the lter diagonalization method FDM A pulse sequence was designed for the optimal correlation of acetyl methyl protons methyl carbons and carbonyl carbons The multi dimensional nature of the FDM coupled with the advantages of constant time evolution periods resulted in marked improvements over Fourier transform FT and mirrorimage linear prediction MI LP processing methods The three methods were directly compared using identical data sets A highly resolved 3D spectrum was achieved with the FDM using a very short experimental time 28 min 2004 Elsevier Inc All rights reserved Keywords Filter diagonalization method Multi dimensional NMR Constant time C 13 labeling O acetylation Oligosaccharides 1 Introduction In the quest to provide detailed structural and dynamic information about macromolecules of ever larger size and complexity the greatest single limitation in NMR spectroscopy is the overlap of cross peaks At some upper size limit the assignment of many signals and deduction of their associated spin systems simply becomes impossible Procedures for diminishing cross peak area or volume such as decoupling in indirect or direct dimensions tROSY 1 or extracting singlet spectra using



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