Two-dimensional NMR studies of native coenzyme F430

Modern two-dimensional (2D) NMR spectroscopic methods are used to determine signal assignments and structural features of the recently discovered nickel(II)-containing coenzyme F430. This is the first detailed {sup 1}H and {sup 13}C NMR study of the native form of coenzyme F430. With the use of COSY...

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Bibliographic Details
Published in:Journal of the American Chemical Society 1990-03, Vol.112 (6), p.2178-2184
Main Authors: Won, Hoshik, Summers, Michael F, Olson, Karl D, Wolfe, Ralph S
Format: Article
Language:English
Subjects:
550500 - Metabolism
BACTERIA
BASIC BIOLOGICAL SCIENCES
Biological and medical sciences
COENZYMES
DATA
DATA ANALYSIS
EXPERIMENTAL DATA
Fundamental and applied biological sciences. Psychology
INFORMATION
MAGNETIC RESONANCE
MEASURING INSTRUMENTS
MEASURING METHODS
METHANOGENIC BACTERIA
MICROORGANISMS
Molecular biophysics
NUCLEAR MAGNETIC RESONANCE
NUMERICAL DATA
RESONANCE
Spectroscopy : techniques and spectras
STRUCTURAL CHEMICAL ANALYSIS
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Summary:Modern two-dimensional (2D) NMR spectroscopic methods are used to determine signal assignments and structural features of the recently discovered nickel(II)-containing coenzyme F430. This is the first detailed {sup 1}H and {sup 13}C NMR study of the native form of coenzyme F430. With the use of COSY, HOHAHA, NOESY, and ROESY {sup 1}H-{sup 1}H correlated spectroscopies in combination with HMQC and HMBC {sup 1}H-{sup 13}C correlated spectroscopies, signal assignments were made for all carbon atoms and nonexchangeable protons. The data confirm 16 of the 21 specific {sup 13}C NMR signal assignments made earlier for native F430 by classical 1D NMR methods and provide assignment (or reassignment) of the remaining carbon atoms. The {sup 1}H NMR signal assignments reported here are in good agreement with the partial assignments reported previously for the pentamethyl ester derivative of F430 (F430M) in CD{sub 2}Cl{sub 2} solution. In addition, long-range through-bond {sup 1}H-{sup 13}C connectivities confirm aspects of the F430 structure deduced from studies of F430M by traditional spectroscopic and chemical methods.
ISSN:0002-7863
1520-5126
DOI:10.1021/ja00162a020