Bryan's Literature Update for January 8, 2009

Here comes the fun!

(Note the noteworthy submissions from Dr. Luke O'Dell in this wrap-up.)

These are the journals that were exhaustively combed (three times over. Honestly.) to procure the following entries:

Advanced Mater. (Wiley)
Chem. Phys. Lett. (Elsevier)
Chem. Commun. (RSC)
Dalton Trans. (RSC)

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Chemical Physics Letters
Vol: 458, Issue: 4-6, June 17, 2008
pp. 368-372

Title: Intermolecular multiple-quantum coherences between spin 1/2 and quadrupolar nuclei in liquid nuclear magnetic resonance
Authors: Chen, S.; Cai, S.; Chen, Z.
Abstract (English): The features of the NMR signals from intermolecular multiple-quantum coherences between spin 1/2 and quadrupolar nuclei were investigated theoretically and experimentally.

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Chemical Physics Letters
Vol: 458, Issue: 4-6, June 17, 2008
pp. 391-395

Title: Improving resolution in proton solid-state NMR by removing nitrogen-14 residual dipolar broadening
Authors: Stein, R.S.; Elena, B.; Emsley, L.
Abstract (English): Improved resolution is obtained for 1H solid-state NMR spectra by removing residual broadening due to interactions with neighboring 14N nuclei.

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Chemical Physics Letters
Vol: 459, Issue: 1-6, June 27, 2008
pp. 188-193

Title: Solid-state single-scan 2D NMR under magic-angle-spinning
Authors: Gal, M.; Melian, C.; Demco, D.E.; Blumich, B.; Frydman, L.
Abstract (English): 2D NMR rubber spectrum collected within a single-scan (27ms total time) using a 2ms mixing time and magic-angle-spinning at 17kHz.

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Chemical Physics Letters
Vol: 460, Issue: 1-3, July 20, 2008
pp. 278-283

Title: MIRROR recoupling and its application to spin diffusion under fast magic-angle spinning
Authors: Scholz, I.; Huber, M.; Manolikas, T.; Meier, B.H.; Ernst, M.
Abstract (English): A new second-order recoupling experiment under MAS NMR conditions is introduced. It allows measurement of proton-driven spin-diffusion spectra even at fast MAS conditions.

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Chemical Physics Letters
Vol: 460, Issue: 4-6, July 30, 2008
pp. 531-535

Title: Simultaneous adiabatic spin-locking cross polarization in solid-state NMR of paramagnetic complexes
Authors: Peng, W.K.; Samoson, A.; Kitagawa, M.
Abstract (English): 13C NMR spectrum of Cu(II)(d,l-alanine)2.H2O, observed with different techniques, (a) SADIS cross polarization, (b) RAMP cross polarization, and (c) direct excitation of 13C. The signal-to-noise ratios (SNRs) are denoted besides its peaks.

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Chemical Physics Letters
Vol: 461, Issue: 1-3, August 8, 2008
pp. 33-37

Title: From correlation-consistent to polarization-consistent basis sets estimation of NMR spin-spin coupling constant in the B3LYP Kohn-Sham basis set limit
Author: Kupka, T.
Abstract (English): Based on recently B3LYP calculated spin-spin coupling constants (SSCC) of several small molecules with cc-pVxZ, cc-pCVxZ, cc-pCVxZ-sd and cc-pCVxZ-sd+t basis sets, a reasonably fit, using the two-parameter formula, to the complete basis set limit (CBS) is shown. Calculation of water's ^1J(OH) using B3LYP/cc-pCVxZ and B3LYP/pcJ-n significantly improved the FC term and its total convergence.

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Chemical Physics Letters
Vol: 462, Issue: 1-3, September 1, 2008
pp. 125-128

Title: Quantification of cross polarization with relaxation compensated reciprocity relation in NMR
Authors: Shu, J.; Chen, Q.; Zhang, S.
Abstract (English): Computer simulated reciprocity relation between the dynamics of cross polarization (CP) and cross depolarization (CDP) for a powder sample under fast magic angle spinning (MAS=40kHz). The symmetrical pattern between CP(t) and CDP(t) manifests the quantification of cross polarization under fast MAS. In the simulation, the dipolar coupling constant for a 1H-13C spin pair is d=25.37kHz and the RF spin-locking fields f1I and f1S are 140 and 100kHz, respectively.

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Chemical Physics Letters
Vol: 463, Issue: 4-6, October 1, 2008
pp. 418-421

Title: Determination of transverse relaxation rates of individual spins while quenching echo modulations due to homonuclear scalar couplings
Authors: Aeby, N.; Bodenhausen, G.
Abstract (English): When spin-echo modulations are quenched, individual transverse relaxation rate constants R2(I)=1/T2(I) can be determined for each spin I individually site by site.

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Chemical Physics Letters
Vol: 464, Issue: 1-3, October 13, 2008
pp. 97-102

Title: QCPMG using adiabatic pulses for faster acquisition of ultra-wideline NMR spectra
Authors: O'Dell, L.A.; Schurko, R.W.
Abstract (English): A QCPMG-like pulse sequence utilizing adiabatic (WURST) pulses. This sequence allows broadband excitation of ultra-wideline solid-state NMR spectra, combined with a significant increase in signal per scan. The sequence has been successfully used to acquire 71Ga and 91Zr spectra over 500kHz in width without any frequency or field adjustment. It can also be used to observe satellite transitions.

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Chemical Physics Letters
Vol: 464, Issue: 1-3, October 13, 2008
pp. 42-48

Title: New perspectives on calcium environments in inorganic materials containing calcium-oxygen bonds: A combined computational-experimental ^4^3Ca NMR approach
Authors: Gervais, C.; Laurencin, D.; Wong, A.; Pourpoint, F.; Labram, J.; Woodward, B.; Howes, A.P.; Pike, K.J.; Dupree, R.; Mauri, F.; Bonhomme, C.; Smith, M.E.
Abstract (English): The potential of a combined experimental-computational 43Ca solid state NMR approach for the structural analysis of inorganic compounds is presented.

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Chemical Physics Letters
Vol: 464, Issue: 4-6, October 23, 2008
pp. 235-239

Title: Irreducible spherical tensor analysis of quadrupolar nuclei
Authors: Chandra Shekar, S.; Rong, P.; Jerschow, A.
Abstract (English): Selection of a specific spherical tensor term from the density matrix of a spin=7/2 particle, demonstrated experimentally as a function of evolution time.

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Chemical Physics Letters
Vol: 466, Issue: 1-3, November 24, 2008
pp. 95-99

Title: Homonuclear dipolar decoupling at magic-angle spinning frequencies up to 65kHz in solid-state nuclear magnetic resonance
Authors: Leskes, M.; Steuernagel, S.; Schneider, D.; Madhu, P.K.; Vega, S.
Abstract (English): Experimental aspects of the implementation of homonuclear dipolar decoupling schemes for 1H spectroscopy in solid-state NMR at high magic-angle spinning frequencies of up to 65kHz are demonstrated.

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Chemical Physics Letters
Vol: 466, Issue: 4-6, December 4, 2008
pp. 227-234

Title: Application of static microcoils and WURST pulses for solid-state ultra-wideline NMR spectroscopy of quadrupolar nuclei
Authors: Tang, J.A.; O'Dell, L.A.; Aguiar, P.M.; Lucier, B.E.G.; Sakellariou, D.; Schurko, R.W.
Abstract (English): The uses of microcoils and WURST pulses for acquiring ultra-wideline (UW) NMR spectra of half-integer quadrupolar nuclei are explored.

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Chemical Physics Letters
Vol: 466, Issue: 4-6, December 4, 2008
pp. 247-251

Title: Efficient heteronuclear decoupling by quenching rotary resonance in solid-state NMR
Authors: Weingarth, M.; Tekely, P.; Bodenhausen, G.
Abstract (English): We propose efficient heteronuclear decoupling by quenching rotary resonance in fast MAS solid-state NMR

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Chem. Commun.
2008, 5568 - 5570,
DOI: 10.1039/b812928b


Title: Quantifying the fraction of glycine and alanine in -sheet and helical conformations in spider dragline silk using solid-state NMR

Authors: Gregory P. Holland, Janelle E. Jenkins, Melinda S. Creager, Randolph V. Lewis and Jeffery L. Yarger

Abstract: Solid-state two-dimensional refocused INADEQUATE MAS NMR experiments resolve distinct helical and -sheet conformational environments for both alanine and glycine in Nephila clavipes dragline silk fibers; the fraction of alanine and glycine in -sheet structures is determined to be 82% ± 4% and 28% ± 5%, respectively.

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Chem. Commun.
2008, 5722 - 5724
DOI: 10.1039/b812905c

Title: Deuterated polymer gels for measuring anisotropic NMR parameters with strongly reduced artefacts

Authors: Grit Kummerlöwe, Sebastian Knör, Andreas O. Frank, Thomas Paululat, Horst Kessler and Burkhard Luy

Abstract: Perdeuterated poly(styrene) is introduced as an almost artefact-free and arbitrarily scalable alignment medium for measuring residual dipolar couplings and other anisotropic NMR parameters; the spectral quality achievable in this new medium is demonstrated for HSQC spectra leading to the conformational analysis of staurosporine and homonuclear TOCSY-type experiments.

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Chem. Commun.
2008, 5933 - 5935
DOI: 10.1039/b814326a

Title: Solid-state 115In NMR study of indium coordination complexes

Authors: Fu Chen, Guibin Ma, Ronald G. Cavell, Victor V. Terskikh and Roderick E. Wasylishen

Abstract: The feasibility of solid-state 115In NMR studies is demonstrated by an examination of four different coordination complexes: indium(III) acetylacetonate, indium(III) tris(tropolonato), indium(III) triiodide bis(tris(4-methoxyphenyl)phosphine oxide) and indium(III) trichloride tris(2,4,6-trimethoxyphenyl)phosphine. The results provide information about the electric field gradients and magnetic shielding at the indium nuclei through the nuclear quadrupolar and chemical shift parameters, respectively. The CQ values in these four complexes range between 106.0 ± 2.0 and 200.0 ± 4.0 MHz, while the magnetic shielding anisotropies fall in the range from 85 ± 15 to 550 ± 60 ppm. Finally, this research demonstrates that solid-state 115In NMR studies are facilitated by performing experiments at the highest possible magnetic-field strengths, and that NMR offers a promising tool for the characterization of indium compounds.

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Chem. Commun.
2008, 5981 - 5983
DOI: 10.1039/b813237b

Title: Revealing molecular self-assembly and geometry of non-covalent halogen bonding by solid-state NMR spectroscopy

Authors: Markus Weingarth, Noureddine Raouafi, Benjamin Jouvelet, Luminita Duma, Geoffrey Bodenhausen, Khaled Boujlel, Bernd Schöllhorn and Piotr Tekely

Abstract: We report a new spectroscopic fingerprint of intermolecular contacts in halogen bond-driven self-assembling aggregates and a precise determination of intermolecular NI distances in microcrystalline samples.

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Chem. Commun.
2009, 186 - 188
DOI: 10.1039/b817017g

Title: A natural abundance 33S solid-state NMR study of layered transition metal disulfides at ultrahigh magnetic field

Authors: Andre Sutrisno, Victor V. Terskikh and Yining Huang

Abstract: Using a series of layered transition metal disulfides we demonstrate that the wide-line natural abundance solid-state NMR spectra of 33S in a less symmetric environment can readily be obtained at ultrahigh magnetic field of 21.1 T and that surprisingly these closely related materials display a wide range of 33S quadrupole coupling constant and chemical shift anisotropy values.

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Dalton Trans.
2008, 3723 - 3728
DOI: 10.1039/b802496k


Title: Structural, 197Au Mössbauer and solid state 31P CP/MAS NMR studies on bis (cis-bis(diphenylphosphino)ethylene) gold(I) complexes [Au(dppey)2]X for X = PF6, I

Authors: Peter C. Healy, Bradley T. Loughrey, Graham A. Bowmaker and John V. Hanna

Abstract: 197Au Mössbauer spectra for the d10 gold(I) phosphine complexes, [Au(dppey)2]X (X = PF6, I; dppey = (cis-bis(diphenylphosphino)ethylene), and the single crystal X-ray structure and solid state 31P CPMAS NMR spectrum of [Au(dppey)2]I are reported here. In [Au(dppey)2]I the AuP4 coordination geometry is distorted from the D2 symmetry observed for the PF6- complex with Au–P bond lengths 2.380(2)–2.426(2) Å and inter-ligand P–Au–P angles 110.63(5)–137.71(8)̊. Quadrupole splitting parameters derived from the Mössbauer spectra are consistent with the increased distortion of the AuP4 coordination sphere with values of 1.22 and 1.46 mm s-1 for the PF6- and I- complexes respectively. In the solid state 31P CP MAS NMR spectrum of [Au(dppey)2]I, signals for each of the four crystallographically independent phosphorus nuclei are observed, with the magnitude of the 197Au quadrupole coupling being sufficiently large to produce a collapse of 1J(Au–P) splitting from quartets to doublets. The results highlight the important role played by the counter anion in the determination of the structural and spectroscopic properties of these sterically crowded d10 complexes.

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Dalton Trans.
2008, 3782 - 3790
DOI: 10.1039/b719526e

Title: Perspectives in paramagnetic NMR of metalloproteins

Authors: Ivano Bertini, Claudio Luchinat, Giacomo Parigi and Roberta Pierattelli

Abstract: NMR experiments and tools for the characterization of the structure and dynamics of paramagnetic proteins are presented here. The focus is on the importance of 13C direct-detection NMR for the assignment of paramagnetic systems in solution, on the information contained in paramagnetic effects observed both in solution and in the solid state, and on novel paramagnetism-based tools for the investigation of conformational heterogeneity in protein–protein complexes or in multi-domain proteins.

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Dalton Trans.
2008, 4965 - 4974
DOI: 10.1039/b803510p

Title: Nitrogen-15 NMR spectroscopy of N-metallated nucleic acids: insights into 15N NMR parameters and N–metal bonds

Authors: Yoshiyuki Tanaka and Akira Ono

Abstract: It was recently demonstrated spectroscopically that RNA/DNA nucleobases can bind to metal cations in aqueous solution through coordination bonds and covalent bonds. Nitrogen-15 (15N) NMR spectroscopy was employed and shown to be a powerful tool for determining the mode of metal ion binding to nitrogen atoms in RNA/DNA molecules. This review describes 15N NMR spectroscopic characteristics in accordance with the mode of metal ion binding to nitrogen atoms. The general rules for 15N chemical shift changes, which are applicable to the determination of the metal ion binding mode of N-metallated compounds, are also described.

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Dalton Trans.
2008, 5296 - 5301
DOI: 10.1039/b809062a

Title: Effect of oxygen content on the 29Si NMR, Raman spectra and oxide ion conductivity of the apatite series, La8+xSr2-x(SiO4)6O2+x/2

Authors: A. Orera, E. Kendrick, D. C. Apperley, V. M. Orera and P. R. Slater

Abstract: 29Si NMR data have been recorded for the apatite series La8+xSr2-x(SiO4)6O2+x/2 (0 x 1.0). For x = 0, a single NMR peak is observed at a chemical shift of -77 ppm, while as the La:Sr ratio and hence interstitial oxygen content is increased, a second peak at a chemical shift of -80 ppm is observed, which has been attributed to silicate groups neighbouring interstitial oxide ions. An increase in the intensity of this second peak is observed with increasing x, consistent with an increase in interstitial oxide ion content, and the data are used to estimate the level of interstitial oxide ions, and hence Frenkel-type disorder in these materials. The increase in second 29Si NMR peak intensity/interstitial oxide ion content is also shown to correlate with an increase in conductivity. The effect of interstitial oxygen content can also be studied by means of Raman spectroscopy, with a new mode at 360 cm-1 appearing for samples with x > 0 in the symmetric bending mode energy region of the SiO4 group. The intensity of this mode increases with increasing oxygen content, yielding results comparable to those from the NMR studies, showing the complementarities of the two techniques.

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Dalton Trans.
2008, 6150 - 6158
DOI: 10.1039/b810863c

Title: Structure determination of -Pb2ZnF6 by coupling multinuclear solid state NMR, powder XRD and ab initio calculations

Authors: Charlotte Martineau, Franck Fayon, Christophe Legein, Jean-Yves Buzaré, Monique Body, Dominique Massiot and François Goutenoire

Abstract: The results from one-dimensional multinuclear (19F, 207Pb and 67Zn) magic-angle spinning nuclear magnetic resonance experiments combined with the use of the ISODISPLACE program allow for the space group determination of -Pb2ZnF6 (no. 138 P42/ncm). The structure was refined from X-ray powder diffraction data (a = 5.633 (1) and c = 16.247 (1) , Z = 4). -Pb2ZnF6 has one six-fold coordinated Zn, one eleven-fold coordinated Pb and five F non-equivalent crystallographic sites and is built from alternated layers parallel to the (a, b) plane; tilted ZnF42- layers of corner sharing ZnF64- octahedra and FPb+ layers of edge sharing FPb47+ tetrahedra. The structure of -Pb2ZnF6 was then optimized using the ab initio code WIEN2k and the calculated 67Zn EFG is in agreement with the NMR results. 19F–19F proximities and 19F–207Pb connectivities were evidenced using through-space and through-bond NMR correlation experiments, respectively, and support the proposed structure. 19F–207Pb J-coupling was also used to select fluorine resonances depending on the number of neighbouring lead ions, leading to an unambiguous assignment of the different 19F resonances.

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