Double quantum solid-state NMR

Levitt et al.69 have used the double quantum solid state NMR in the studies of bond lengths for a series of five 13C labelled samples of rhodopsin. On the basis of DQ-filtered signal trajectories and numerical spin simulations of the signal points, the through-space dipole-dipole coupling between neighbouring 13C nuclei has been estimated. Estimated dipole-dipole couplings have been converted into the intemuclear distances (Table 2) [32],... 

K. Schmidt-Rohr, A double-quantum solid-state NMR technique for determining torsion angles in polymers. Macromolecules, 1996, 29, 3975-3981. 

Most recently, a double-quantum solid-state NMR technique has been reported [47]. This gives detailed structural information such as torsion angles for unoriented amorphous polymers including unoriented polypeptides with NMR tensor correlation in the labeled segments. This new solid-... 

Concistre M, Gansmiiller A, McLean N et al (2009) Light penetration and photoisomerization in rhodopsin studied by numerical simulations and double-quantum solid-state NMR spectroscopy. J Am Chem Soc 131 6133-6140... 

Carravetta M, Zhao X, Johannessen OG et al (2004) Protein-induced bonding perturbation of the rhodopsin chromophore detected by double-quantum solid-state NMR. J Am Chem Soc... 

R 15 D.M. Jonas, Two-Dimensional Femtosecond Spectroscopy , p. 425 R 16 G.P. Drobny, J.R. Long, T. Karlsson, W. Shaw, J. Popham, N. Oyler, P. Bower, J. Stringer, D. Gregory, M. Mehta and P.S. Stayton, Structural Studies of Biomaterials Using Double-Quantum Solid-State NMR Spectroscopy , p. 531... 

Structural studies of biomaterials using double quantum solid state NMR have been reviewed by Drobny et al. Both the theory and practice of doublequantum solid state NMR techniques for determining the secondary structures of surface-adsorbed peptides and proteins are presented. In particular, the use of solid state NMR dipolar techniques to provide the high-resolution structural and dynamic characterisation of a hydrated biomineralisation protein, salivary statherin, adsorbed to its biologically relevant hydroxyapatite surface is presented. This article also reviews NMR data on peptides designed to adsorb from aqueous solutions onto highly porous hydrophobic surfaces with specific helical secondary structures. 

Brouwer, D. H., Alavi, S., Ripmeester, J. A., A double quantum Xe-129 NMR experiment for probing xenon in multiply-occupied cavities of solid-state inclusion compounds. Phys. Chem. Chem. Phys. 2007, 9, 1093-1098. 

ID IQ 2D 2D-NMR 2h2o 2Q 3Q 9BEN A1 ABS AC ACM ACN AFM Al-CSM ALMA-i5 Al-m-EPDM AN AO APT ASTM ATR ATR-IR B/S BABA Two-dimensional Single-quantum One-dimensional Deuteron solid-state NMR Deuterated water Double-quantum Triple-quantum 9 borobicyclo [3, 3, 1] nonane Amide 1 Acrylonitrile-butadiene-styrene terpolymer Accelerator Acrylate rubber Acrylonitrile Atomic Force Microscopy Aluminium salt of chlorosulfonate polyethylene Allyl-rf5 methacrylate Aluminium salt of maleated EPDM Acrylonitrile 1-Allyl oxyoctane Attached Proton Test American Standards for Testing and Materials Attenuated total reflectance spectroscopy Attenuated total reflectance-IR spectroscopy Butadiene/styrene Back-to-back... 

Solid-state NMR spectroscopy has been demonstrated as a well established technique for characterization of zeolites and other porous materials with respect to structure elucidation, pore architecture, catalytic behaviour and mobility properties. The latest progress in the development of NMR techniques, both with respect to software and hardware improvements, has contributed to the present state of the art for NMR within the field of characterization of zeolitic materials. Furthermore, the introduction of NMR imaging (110), two-dimensional quintuple-quantum NMR spectroscopy (111) and transfer of populations in double resonance (TRAPDOR) NMR (112,113) will extent the horizons of zeolite characterization science. As a final example, the Al => Si TEDOR experiment directly proves, for the first time, that silicon substitutes for phosphorous atoms in the framework of SAPO-37 (114). The Al... 

In the last few years the combination of high spinning speed with 2D multiple quantum spectroscopy has opened up new possibilities in the area of hydrogen bond investigation by 1H solid state NMR. The field has been exhaustively reviewed by Schnell and Spiess [77]. In Fig. 3.2.26 is reported, for example, the information available by ID and 2D double quantum proton spectra in the case of malonic acid. Each signal can be unequivocally assigned to the respective proton, and the chemical shift of the carboxylic protons can be correlated to the 0-0 distance. Furthermore the intermolecular correlation between CH2 and COOH protons can be used as a constraint for establishing the conformation and array structure in the solid state. 

Solid state NMR methods for the determination of intemuclear dipole-dipole couplings between homonuclear spin-1/2 nuclei have been presented by Gunne. " The methods considered are suitable for relatively dense dipolar networks which are still dominated by two-spin interactions. Symmetry derived pulse sequences with improved compensation against chemical shift anisotropies were found assuming a small isotropic chemical shift difference and using numerical calculations of the spin dynamics. It has been shown that a constant time procedure can be used to acquire reliable double quantum build up curves even in systems in which damping obscures oscillations in their symmetric build up curve. This technique has been demonstrated on four crystalline model com-... 

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