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Solid State Nuclear Magnetic Resonance

Sylvian Cadars, Nak Ho Ahn, Kirill Okhotnikov, Jiho Shin, Aurélie Vicente, Suk Bong Hong, Christian Fernandez
Atomic substitutions are a central feature of the physicochemical properties of an increasing number of solid-state materials. The complexity that this chemical disorder locally generates in otherwise crystalline solids poses a major challenge to the understanding of the relationships between the structure and properties of materials at the atomic and molecular level. Strategies designed to efficiently explore the ensemble of local chemical environments present in disordered crystals and predict their signatures in local spectroscopies such as solid-state nuclear magnetic resonance (NMR) are therefore essential...
April 13, 2017: Solid State Nuclear Magnetic Resonance
Amrit Venkatesh, Michael P Hanrahan, Aaron J Rossini
Fast magic angle spinning (MAS) and proton detection has found widespread application to enhance the sensitivity of solid-state NMR experiments with spin-1/2 nuclei such as (13)C, (15)N and (29)Si, however, this approach is not yet routinely applied to half-integer quadrupolar nuclei. Here we have investigated the feasibility of using fast MAS and proton detection to enhance the sensitivity of solid-state NMR experiments with half-integer quadrupolar nuclei. The previously described dipolar hetero-nuclear multiple quantum correlation (D-HMQC) and dipolar refocused insensitive nuclei enhanced by polarization transfer (D-RINEPT) pulse sequences were used for proton detection of half-integer quadrupolar nuclei...
March 30, 2017: Solid State Nuclear Magnetic Resonance
Hiroki Nagashima, Grégory Tricot, Julien Trébosc, Olivier Lafon, Jean-Paul Amoureux, Frédérique Pourpoint
We report here an original NMR sequence allowing the acquisition of 3D correlation NMR spectra between three distinct heteronuclei, among which two are half-integer spin quadrupolar nuclei. Furthermore, as two of them exhibit close Larmor frequency, this experiment was acquired using a standard triple-resonance probe equipped with a commercial frequency splitter. This NMR technique was tested and applied to sodium alumino-phosphate compounds with (31)P as the spin-1/2 nucleus and (23)Na and (27)Al as the close Larmor frequencies isotopes...
March 22, 2017: Solid State Nuclear Magnetic Resonance
João Medeiros-Silva, Shehrazade Jekhmane, Marc Baldus, Markus Weingarth
(1)H-detected solid-state NMR in combination with (1)H/(2)D exchange steps allows for the direct identification of very strong hydrogen bonds in membrane proteins. On the example of the membrane-embedded potassium channel KcsA, we quantify the longevity of such very strong hydrogen bonds by combining time-resolved (1)H-detected solid-state NMR experiments and molecular dynamics simulations. In particular, we show that the carboxyl-side chain of the highly conserved residue Glu51 is involved in ultra-strong hydrogen bonds, which are fully-water-exposed and yet stable for weeks...
March 18, 2017: Solid State Nuclear Magnetic Resonance
K Seleznyova, N A Sergeev, M Olszewski, P Stępień, S V Yagupov, M B Strugatsky, J Kliava
A comparative analysis of the Czjzek's and Maurer's models of the joint distribution density of NMR quadrupole parameters has been carried out in view of their application to account for spectra broadening induced by local disorder in crystals. As an example of such an application, we have considered Magic Angle Spinning NMR of (11)B and (71)Ga isotopes in polycrystalline gallium borate. Computer simulations carried out using both models unambiguously show that in the case of low local disorder the Maurer's model, in contrast to the Czjzek's model, provides satisfactory fits to experimental NMR spectra...
March 18, 2017: Solid State Nuclear Magnetic Resonance
Koji Kanehashi
Structural roles of Ca in aluminosilicate glasses have been investigated by solid-state (43)Ca, (17)O, and (27)Al NMR spectroscopy. In 15Al2O3-55SiO2-15CaO-15RO (R=Mg, Ca, Sr, and Na2) (mol%) glass systems wherein half of the alkaline plus alkaline-earth cations charge-compensate (AlO4)(‒) tetrahedra and the other half modify the glass network, with decreasing cation field strength (CFS) in the order of Mg(2+)>Ca(2+)>Sr(2+)>Na(+), the isotropic chemical shift (δiso) of (43)Ca moves to a higher frequency and the quadrupolar coupling constant (PQ) of (43)Ca decreases...
March 3, 2017: Solid State Nuclear Magnetic Resonance
Tiago Venâncio, Lyege Magalhaes Oliveira, Javier Ellena, Nubia Boechat, Steven P Brown
Fast magic-angle spinning (MAS) NMR is used to probe intermolecular interactions in a diethylcarbamazine salt, that is widely used as a treatment against adult worms of Wuchereria bancrofti which cause a common disease in tropical countries named filariasis. Specifically, a dihydrogen citrate salt that has improved thermal stability and solubility as compared to the free form is studied. One-dimensional (1)H, (13)C and (15)N and two-dimensional (1)H-(13)C and (14)N-(1)H heteronuclear correlation NMR experiments under moderate and fast MAS together with GIPAW (CASTEP) calculations enable the assignment of the (1)H, (13)C and (14)N/(15)N resonances...
March 2, 2017: Solid State Nuclear Magnetic Resonance
A S Andreev, N V Bulina, M V Chaikina, I Yu Prosanov, V V Terskikh, O B Lapina
In this work, we report the results of a detailed structural study of a promising bioceramic material silicocarnotite Ca5(PO4)2SiO4 (SC) synthesized from mechanochemically treated nanosized silicon-substituted hydroxyapatite by annealing at 1000°C. This novel synthetic approach represents an attractive and efficient route towards large-scale manufacturing of the silicocarnotite-based bioceramics. A combination of solid-state nuclear magnetic resonance (NMR), powder X-ray crystallography and density function theory (DFT) calculations has been implemented to characterize the phase composition of the prepared composite materials and to gain insight into the crystal structure of silicocarnotite...
February 22, 2017: Solid State Nuclear Magnetic Resonance
Lena Marie Funke, Henrik Bradtmüller, Hellmut Eckert
The case of rotational echo double resonance (REDOR) experiments on the observe nuclei (11)B and (31)P interacting with multiple I=1 quadrupolar nuclei is analyzed in detail by SIMPSON simulations and experimental studies. The simulations define the region within the parameter space spanned by nutation frequency, quadrupolar coupling constant and spinning frequency where the parabolic analysis of the initial REDOR curve in terms of dipolar second moments has validity. The predictions are tested by experimental studies on the crystalline model compounds lithium diborate and lithium pyrophosphate, which are subsequently extended to measure dipolar second moments M2((11)B{(6)Li}) and M2((31)P{(6)Li}) in three borophosphate glasses...
February 20, 2017: Solid State Nuclear Magnetic Resonance
Habeeba K Miah, Rosalie Cresswell, Dinu Iuga, Jeremy J Titman
A (1)H anisotropic-isotropic chemical shift correlation experiment which employs symmetry-based recoupling sequences to reintroduce the chemical shift anisotropy in ν1 and ultrafast MAS to resolve (1)H sites in ν2 is described. This experiment is used to measure (1)H shift parameters for L-ascorbic acid, a compound with a relatively complex hydrogen-bonding network in the solid. The (1)H CSAs of hydrogen-bonded sites with resolved isotropic shifts can be extracted directly from the recoupled lineshapes. In combination with DFT calculations, hydrogen positions in crystal structures obtained from X-ray and neutron diffraction are refined by comparison with simulations of the full two-dimensional NMR spectrum...
February 13, 2017: Solid State Nuclear Magnetic Resonance
Paul Jonsen
During August 2015, the author surveyed 76 solid state NMR scientists from materials science to biology, academic to industrial, based in North America, Europe, India, China, Japan and Australia. The subject concerned barriers to the wider acceptance of solid state NMR and included the various barriers based on experimental, funding, vendor based and community aspects. This survey was confidential. However, many of the survey participants requested that at least the results of the part of the survey relevant to our community be made public...
February 9, 2017: Solid State Nuclear Magnetic Resonance
G Tricot, B Doumert, B Revel, M Bria, J Trebosc, H Vezin
Solid state NMR is applied in this contribution on the xAl2O3-(50-x/2)Na2O-(50-x/2)P2O5 composition line (with 0<x<5mol%) in order to investigate the distribution of Al(3+) ions in Al2O3-doped sodium phosphate glasses. The structure was analysed by (i) (27)Al 1D-, 3Q-, DQ- MAS-NMR analysis and (ii) 1D (31)P, (27)Al((31)P) 2D D-HMQC MAS-NMR and 2D (31)P R-INADEQUATE technique. The (27)Al NMR results confirm the presence of six-coordinated aluminate as major aluminate species and indicate that Al(3+) ions are fully dissociated in the glass network...
February 9, 2017: Solid State Nuclear Magnetic Resonance
Günter Hempel
A method is described for the elimination of artefacts that arise in time-domain signals because of the presence of digital and analogous filters. Such artefacts are mostly located at the beginning of the free-induction decay (FID). The procedure introduced here is particularly important if at least one signal component decays rather quickly, i.e. if there is only a small number of data containing this component (as for solid-state (1)H or (2)H FIDs). The method is able to restore the original signal by deconvolution of the spectrometer output from the transfer function of the spectrometer console...
February 3, 2017: Solid State Nuclear Magnetic Resonance
Ming Shen, Qun Chen, Bingwen Hu
(14)N MAS overtone spectroscopy is mainly limited by narrow excitation bandwidths owing to the use of very long pulses to get stronger signals. We previously reported the use of modified 90° composite pulses for broadband excitation in (1)H-{NOTDQ14}D-HMQC experiments at ultra-fast MAS. In this work, we modified the 180° composite pulses, which are originally designed for spin 1/2 nuclei, for both indirect detection in (1)H-{NOTDQ14}D-HMQC experiment and direct detection in one-pulse experiment, and found that the modified 180° composite pulses are useful for broadband excitation...
February 3, 2017: Solid State Nuclear Magnetic Resonance
Yue Zhang, Bryan E G Lucier, Victor V Terskikh, Renlong Zheng, Yining Huang
Ga-MIL-53 is a metal-organic framework (MOF) that exhibits a "breathing effect," in which the pore size and overall MOF topology can be influenced by temperature, pressure, and host-guest interactions. The phase control afforded by this flexible framework renders Ga-MIL-53 a promising material for guest storage and sensing applications. In this work, the structure and behavior of four Ga-MIL-53 phases (as, ht, enp and lt), along with CO2 adsorbed within Ga-MIL-53 at various loading levels, has been investigated using (69/71)Ga solid-state NMR (SSNMR) experiments at 21...
January 31, 2017: Solid State Nuclear Magnetic Resonance
Peter A Beckmann, Joseph M Bohen, Jamie Ford, William P Malachowski, Clelia W Mallory, Frank B Mallory, Andrew R McGhie, Arnold L Rheingold, Gilbert J Sloan, Steven T Szewczyk, Xianlong Wang, Kraig A Wheeler
We report a variety of experiments and calculations and their interpretations regarding methyl group (CH3) rotation in samples of pure 3-methylglutaric anhydride (1), pure 3-methylglutaric acid (2), and samples where the anhydride is slowly absorbing water from the air and converting to the acid [C6H8O3(1) + H2O → C6H10O4(2)]. The techniques are solid state (1)H nuclear magnetic resonance (NMR) spin-lattice relaxation, single-crystal X-ray diffraction, electronic structure calculations in both isolated molecules and in clusters of molecules that mimic the crystal structure, field emission scanning electron microscopy, differential scanning calorimetry, and high resolution (1)H NMR spectroscopy...
January 29, 2017: Solid State Nuclear Magnetic Resonance
Anna Naumova, Carsten Tschierske, Kay Saalwächter
In recent years, the analysis of proton double-quantum NMR build-up curves has become an important tool to quantify anisotropic mobility in different kinds of soft materials such as polymer networks or liquid crystals. In the former case, such data provides a measure of orientation-dependent residual (time-averaged) dipolar couplings arising from anisotropic segmental motions, informing about the length and the state of local stretching of the network chains. Previous studies of macroscopically ordered, i.e...
January 26, 2017: Solid State Nuclear Magnetic Resonance
Piotr Paluch, Natalia Potrzebowska, Agnieszka M Ruppert, Marek J Potrzebowski
In this work for the first time we show the power of solid state NMR spectroscopy in structural analysis of alumina and catalysts supported on the alumina surface employing very fast (60kHz) magic angle spinning (MAS) technique. In the methodological part we demonstrate that under such MAS condition, cross-polarization (CP) from proton to aluminum is an efficient process when a very weak (27)Al RF field is applied. The mechanism of CP transfer and the Hartmann-Hahn (H-H) matching conditions were tested for (27)Al RF fields equal to 3...
January 26, 2017: Solid State Nuclear Magnetic Resonance
D Iuga, P Rossi, J Herzfeld, R G Griffin
Chloride ions play important roles in many chemical and biological processes. This paper investigates the possibility of localizing (35)Cl nuclei using solid-state NMR. It demonstrates that distances shorter than 3.8Å, between (13)C atoms and (35)Cl atoms in 10% uniformly labeled (13)C L-tyrosine·HCl and natural abundance Glycine·HCl can be measured using rotational-echo (adiabatic passage) double-resonance (RE(AP)DOR). Furthermore the effect of quadrupolar interaction on the REDOR/REAPDOR experiment is quantified...
April 2017: Solid State Nuclear Magnetic Resonance
Aneta Woźniak-Braszak
Molecular dynamics of the solid 3-(trifluoromethyl) benzoic acid containing proton (1)H and fluorine (19)F nuclei was explored by the solid-state NMR off - resonance technique. Contrary to the previous experiments the proton nuclei system I relaxed in the off - resonance effective field B→e while fluorine nuclei system S was saturated for short time in comparison to the relaxation time T1I. New cross - relaxation solid - state NMR off - resonance experiments were conducted on a homebuilt pulse spectrometer operating at the on-resonance frequency of 30...
February 2017: Solid State Nuclear Magnetic Resonance
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