Selective Chemical Shift Assignment of Bacteriochlorophyllain Uniformly [13C−15N]-Labeled Light-Harvesting 1 Complexes by Solid-State NMR in Ultrahigh Magnetic Field

2010 ◽  
Vol 114 (18) ◽  
pp. 6207-6215 ◽  
Author(s):  
Anjali Pandit ◽  
Francesco Buda ◽  
Adriaan J. van Gammeren ◽  
Swapna Ganapathy ◽  
Huub J. M. de Groot
Keyword(s):  
Magnetic Field ◽  
Solid State ◽  
Chemical Shift ◽  
Solid State Nmr ◽  
Light Harvesting ◽  
Chemical Shift Assignment ◽  
Selective Chemical ◽  
Ultrahigh Magnetic Field ◽  
Shift Assignment

Selective Chemical Shift Assignment of B800 and B850 Bacteriochlorophylls in Uniformly [13C,15N]-Labeled Light-Harvesting Complexes by Solid-State NMR Spectroscopy at Ultra-High Magnetic Field

2005 ◽  
Vol 127 (9) ◽  
pp. 3213-3219 ◽  
Author(s):  
Adriaan J. van Gammeren ◽  
Francesco Buda ◽  
Frans B. Hulsbergen ◽  
Suzanne Kiihne ◽  
Johan G. Hollander ◽  
...  
Keyword(s):  
Magnetic Field ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
Chemical Shift ◽  
High Magnetic Field ◽  
Solid State Nmr ◽  
Chemical Shift Assignment ◽  
Light Harvesting Complexes ◽  
Selective Chemical ◽  
Shift Assignment

scholarly journals Temperature-Dependent Solid-State NMR Proton Chemical-Shift Values and Hydrogen Bonding

2021 ◽  
Author(s):  
Alexander A. Malär ◽  
Laura A. Völker ◽  
Riccardo Cadalbert ◽  
Lauriane Lecoq ◽  
Matthias Ernst ◽  
...  
Keyword(s):  
Magnetic Field ◽  
Hydrogen Bonding ◽  
Solid State ◽  
Chemical Shift ◽  
Hydrogen Bonds ◽  
Solid State Nmr ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Proton Chemical Shift ◽  
Temperature Dependent

Temperature-dependent NMR experiments are often complicated by rather long magnetic-field equilibration times, for example occurring upon a change of sample temperature. We demonstrate that the fast temporal stabilization of the magnetic field can be achieved by actively stabilizing the temperature which allows to quantify the weak temperature dependence of the proton chemical shift which can be diagnostic for the presence of hydrogen bonds. Hydrogen bonding plays a central role in molecular recognition events from both fields, chemistry and biology. Their direct detection by standard structure determination techniques, such as X-ray crystallography or cryo-electron microscopy, remains challenging due to the difficulties of approaching the required resolution, on the order of 1 Å. We herein explore a spectroscopic approach using solid-state NMR to identify protons engaged in hydrogen bonds and explore the measurement of proton chemical-shift temperature coefficients. Using the examples of a phosphorylated amino acid and the protein ubiquitin, we show that fast Magic-Angle Spinning (MAS) experiments at 100 kHz yield sufficient resolution in proton-detected spectra to quantify the rather small chemical-shift changes upon temperature variations.<br>

A natural abundance33S solid-state NMR study of layered transition metaldisulfides at ultrahigh magnetic field

2009 ◽  
pp. 186-188 ◽  
Author(s):  
Andre Sutrisno ◽  
Victor V. Terskikh ◽  
Yining Huang
Keyword(s):  
Magnetic Field ◽  
Solid State ◽  
Solid State Nmr ◽  
Nmr Study ◽  
Ultrahigh Magnetic Field

Combined 135/137Ba Solid-State NMR at an Ultrahigh Magnetic Field and Computational Study of β-Barium Borate

2009 ◽  
Vol 113 (50) ◽  
pp. 21196-21201 ◽  
Author(s):  
Andre Sutrisno ◽  
Cheng Lu ◽  
R. H. Lipson ◽  
Yining Huang
Keyword(s):  
Magnetic Field ◽  
Solid State ◽  
Solid State Nmr ◽  
Computational Study ◽  
Barium Borate ◽  
Ultrahigh Magnetic Field

scholarly journals Exploring the limits of 73Ge solid-state NMR spectroscopy at ultrahigh magnetic field

2010 ◽  
Vol 46 (16) ◽  
pp. 2817 ◽  
Author(s):  
Andre Sutrisno ◽  
Margaret A. Hanson ◽  
Paul A. Rupar ◽  
Victor V. Terskikh ◽  
Kim M. Baines ◽  
...  
Keyword(s):  
Magnetic Field ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
Solid State Nmr ◽  
Solid State Nmr Spectroscopy ◽  
Ultrahigh Magnetic Field

Single Crystal Solid-State NMR of Magnetically Oriented Powder

2014 ◽  
Vol 70 (a1) ◽  
pp. C1086-C1086
Author(s):  
Ryosuke Kusumi ◽  
Fumiko Kimura ◽  
Tsunehisa Kimura
Keyword(s):  
Magnetic Field ◽  
Solid State ◽  
Chemical Shift ◽  
Single Crystal ◽  
Solid State Nmr ◽  
Chemical Shift Tensor ◽  
Magic Angle ◽  
Full Information ◽  
Crystal Rotation ◽  
Rotation Method

Solid-state NMR spectroscopy is one of the most widely used methods for investigating crystal structures, along with the X-ray and neutron diffraction methods. Solid-state NMR can provide structural information including isotropic chemical shift, dipolar and quadrupolar couplings, spin diffusion, and chemical shift tensor. Among these, the chemical shift tensor is of particular significance because the electronic environment around a nucleus is directly reflected on the chemical shift tensor. However, full information of the chemical shift tensor, including principal values and axes, is difficult to obtain experimentally because a large single crystal is required for the measurement. On the other hand, we have proposed the use of a magnetically oriented microcrystal array (MOMA) as an alternative to a single crystal.[1,2] A MOMA is a composite in which microcrystals are aligned three-dimensionally, prepared by using a time-dependent magnetic field. We recently demonstrated that the13C chemical shift tensors of L-alanine crystal can be completely determined by application of the standard procedure in the single-crystal rotation method to a MOMA of L-alanine microcrystals,[3] as shown in Figure 1. The L-alanine MOMA produces sharp resonance peaks without resolution enhancement by magic angle spinning (MAS). In addition, we observed that the positions of the13C resonance peaks vary systematically as a function of the angle ψ that is the sample-rotation angle about the axis inclined by the magic angle with respect to the NMR magnetic field. From the ψ-dependence of the chemical shifts,13C chemical shift tensor was completely determined. We confirmed that the combination of MOMA with the single-crystal rotation method can be applied to other nuclei such as31P and15N. These results clearly show that the MOMA method is a powerful tool for obtaining full information of the chemical shift tensor from a microcrystalline powder without MAS.

scholarly journals 17 O solid‐state NMR at ultrahigh magnetic field of 35.2 T: Resolution of inequivalent oxygen sites in different phases of MOF MIL‐53(Al)

2021 ◽  
Author(s):  
Vinicius Martins ◽  
Jun Xu ◽  
Ivan Hung ◽  
Zhehong Gan ◽  
Christel Gervais ◽  
...  
Keyword(s):  
Magnetic Field ◽  
Solid State ◽  
Solid State Nmr ◽  
Ultrahigh Magnetic Field

scholarly journals Temperature-Dependent Solid-State NMR Proton Chemical-Shift Values and Hydrogen Bonding

2021 ◽  
Author(s):  
Alexander A. Malär ◽  
Laura A. Völker ◽  
Riccardo Cadalbert ◽  
Lauriane Lecoq ◽  
Matthias Ernst ◽  
...  
Keyword(s):  
Magnetic Field ◽  
Hydrogen Bonding ◽  
Solid State ◽  
Chemical Shift ◽  
Hydrogen Bonds ◽  
Solid State Nmr ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Proton Chemical Shift ◽  
Temperature Dependent

Temperature-dependent NMR experiments are often complicated by rather long magnetic-field equilibration times, for example occurring upon a change of sample temperature. We demonstrate that the fast temporal stabilization of the magnetic field can be achieved by actively stabilizing the temperature which allows to quantify the weak temperature dependence of the proton chemical shift which can be diagnostic for the presence of hydrogen bonds. Hydrogen bonding plays a central role in molecular recognition events from both fields, chemistry and biology. Their direct detection by standard structure determination techniques, such as X-ray crystallography or cryo-electron microscopy, remains challenging due to the difficulties of approaching the required resolution, on the order of 1 Å. We herein explore a spectroscopic approach using solid-state NMR to identify protons engaged in hydrogen bonds and explore the measurement of proton chemical-shift temperature coefficients. Using the examples of a phosphorylated amino acid and the protein ubiquitin, we show that fast Magic-Angle Spinning (MAS) experiments at 100 kHz yield sufficient resolution in proton-detected spectra to quantify the rather small chemical-shift changes upon temperature variations.<br>

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