2-Fluoro-ATP, a fluorinated ATP analog. 19F nuclear magnetic resonance studies of the 2-fluoro-ADP∙myosin subfragment-1 complex

1983 ◽  
Vol 61 (2-3) ◽  
pp. 115-119 ◽  
Author(s):  
John H. Baldo ◽  
Poul E. Hansen ◽  
John W. Shriver ◽  
Brian D. Sykes
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Adenine Nucleotides ◽  
Nmr Studies ◽  
Adenine Ring ◽  
Myosin Subfragment ◽  
Myosin Subfragment 1 ◽  
Nmr Properties ◽  
Principal Elements ◽  
Nuclear Magnetic

The synthesis of a fluorinated ATP analog, 2-fluoro-ATP (2-flATP), is described. This analog is designed for 19F nuclear magnetic resonance (NMR) studies of large enzymes and proteins which bind adenine nucleotides. 2-flATP is shown to be active as an ATP analog in a number of enzyme systems, and its 19F-NMR properties are determined. Specifically the principal elements of the 19F-NMR chemical shift tensor are shown to be 104, 12, and −116 ppm. The complex between 2-flADP and the myosin subfragment-1 ATPase is studied by 19FNMR, comparing the normal Michaelis complex and 2-flADP "trapped" on subfragment-1. These complexes are shown to be indistinguishable from the standpoint of the environment and mobility of the adenine ring.

Nuclear magnetic resonance (NMR) studies of sintering effects on the lithium ion dynamics in Li1.5Al0.5Ti1.5(PO4)3

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Edda Winter ◽  
Philipp Seipel ◽  
Tatiana Zinkevich ◽  
Sylvio Indris ◽  
Bambar Davaasuren ◽  
...  
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Lithium Ion ◽  
Magic Angle Spinning ◽  
Spin Lattice Relaxation ◽  
Magic Angle ◽  
Nmr Studies ◽  
Lithium Ions ◽  
Jump Dynamics ◽  
Nuclear Magnetic

Abstract Various nuclear magnetic resonance (NMR) methods are combined to study the structure and dynamics of Li1.5Al0.5Ti1.5(PO4)3 (LATP) samples, which were obtained from sintering at various temperatures between 650 and 900 °C. 6Li, 27Al, and 31P magic angle spinning (MAS) NMR spectra show that LATP crystallites are better defined for higher calcination temperatures. Analysis of 7Li spin-lattice relaxation and line-shape changes indicates the existence of two species of lithium ions with clearly distinguishable jump dynamics, which can be attributed to crystalline and amorphous sample regions, respectively. An increase of the sintering temperature leads to higher fractions of the fast lithium species with respect to the slow one, but hardly affects the jump dynamics in either of the phases. Specifically, the fast and slow lithium ions show jumps in the nanoseconds regime near 300 and 700 K, respectively. The activation energy of the hopping motion in the LATP crystallites amounts to ca. 0.26 eV. 7Li field-gradient diffusometry reveals that the long-range ion migration is limited by the sample regions featuring slow transport. The high spatial resolution available from the high static field gradients of our setup allows the observation of the lithium ion diffusion inside the small (<100 nm) LATP crystallites, yielding a high self-diffusion coefficient of D = 2 × 10−12 m2/s at room temperature.

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