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Crystals
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NMR Crystallography
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NMR Crystallography

A special issue of Crystals (ISSN 2073-4352). This special issue belongs to the section "Crystal Engineering".

Deadline for manuscript submissions: closed (30 June 2019) | Viewed by 21382

Special Issue Editor

Dr. Thomas Bräuniger

E-Mail Website
Guest Editor
Department of Chemistry (Inorganic Chemistry), University of Munich, Munich, Germany
Interests: NMR of single crystals: interaction tensor determination; NMR of quadrupolar nuclei: methods and application; NMR of inorganic compounds: elucidation of structure and dynamics

Special Issue Information

Dear Colleagues,

The fact that Nuclear Magnetic Resonance (NMR) Spectroscopy is capable of supplying valuable information on structure and dynamics of solid materials has been realized since the very early days. In many instances, this NMR-derived information is complementary to that obtained from diffraction methods, but may well extend beyond it, as in applications to non-periodic systems, quantification of local disorder and dynamics, etc.

The term “NMR Crystallography” has been used to describe numerous approaches of NMR-aided structure determination, validation, and refinement. Progress in distance-measuring methodology via dipolar couplings, as well as in multi-dimensional correlation techniques, has made it possible to attempt structure determination solely based on NMR data. The combination of these NMR methods with quantum mechanical structure calculations, which in recent years became increasingly efficient and accurate, has led to a strong increase in publications on such de novo structure determinations by NMR, culminating in the establishment of a “Commission on NMR Crystallography and Related Methods” in the International Union of Crystallography in 2014.

The Special Issue on “NMR Crystallography” in the open access periodical Crystals is a great opportunity to inform a potentially wide audience about the possibilities and successes of this technique. To this end, we invite the submission of papers dealing with “NMR Crystallography” in its broadest sense, in the hope to cover as many aspects of this exciting application of NMR spectroscopy as possible.

Dr. Thomas Bräuniger
Guest Editor

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Crystals is an international peer-reviewed open access monthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2100 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • Structure determination, validation and refinement by NMR crystallography
  • Application of NMR crystallography to inorganic and molecular materials
  • Structural information by combining NMR results with DFT calculations
  • Characterization of dynamic processes in solids by NMR spectroscopy

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Published Papers (5 papers)

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Research

10 pages, 1860 KiB  
Article
NMR Crystallography at Fast Magic-Angle Spinning Frequencies: Application of Novel Recoupling Methods
by Mukul G. Jain, Kaustubh R. Mote and Perunthiruthy K. Madhu
Crystals 2019, 9(5), 231; https://doi.org/10.3390/cryst9050231 - 29 Apr 2019
Cited by 13 | Viewed by 3464
Abstract
Chemical characterisation of active pharmaceutical compounds can be challenging, especially when these molecules exhibit tautomeric or desmotropic behaviour. The complexity can increase manyfold if these molecules are not susceptible to crystallisation. Solid-state NMR has been employed effectively for characterising such molecules. However, characterisation [...] Read more.
Chemical characterisation of active pharmaceutical compounds can be challenging, especially when these molecules exhibit tautomeric or desmotropic behaviour. The complexity can increase manyfold if these molecules are not susceptible to crystallisation. Solid-state NMR has been employed effectively for characterising such molecules. However, characterisation of a molecule is just a first step in identifying the differences in the crystalline structure. 1 H solid-state Nuclear Magnetic Resonance (ssNMR) studies on these molecules at fast magic-angle-spinning frequencies can provide a wealth of information and may be used along with ab initio calculations to predict the crystal structure in the absence of X-ray crystallographic studies. In this work, we attempted to use solid-state NMR to measure 1 H - 1 H distances that can be used as restraints for crystal structure calculations. We performed studies on the desmotropic forms of albendazole. Full article
(This article belongs to the Special Issue NMR Crystallography)
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11 pages, 5701 KiB  
Article
A Preview of a Construction of a Crystal Lattice Based on Intermolecular Interactions
by Vladimír Hejtmánek, Martin Dračínský and Jan Sýkora
Crystals 2019, 9(3), 159; https://doi.org/10.3390/cryst9030159 - 19 Mar 2019
Viewed by 3251
Abstract
A general procedure of crystal packing reconstruction using a certain number of intermolecular interactions is introduced and demonstrated on the crystal structure of l-histidine·HCl·H2O. Geometric restrictions based on intermolecular interactions are used for formation of a molecular pair as a [...] Read more.
A general procedure of crystal packing reconstruction using a certain number of intermolecular interactions is introduced and demonstrated on the crystal structure of l-histidine·HCl·H2O. Geometric restrictions based on intermolecular interactions are used for formation of a molecular pair as a basic repetitive motif of the crystal packing. The geometric restrictions were applied gradually within a supervised procedure, narrowing the scope of possible arrangement of two adjacent molecules. Subsequently, a pair of histidine molecules was used for construction of a molecular chain. The chain formed contained translation information on histidine molecules in one dimension, which coincided with one of the cell parameters. Furthermore, the periodicity in the second and third dimensions can be accomplished by chain assembly into sheets (2D), and sheets can be arranged into the final 3D structure. For this purpose, the rest of the available intermolecular interactions could be used to control the mutual assembly of molecular chains and sheets. Complete molecular packing would enable derivation of standard crystallographic parameters that can be used for verification of the structural model obtained. However, the procedure described for construction of the whole 3D structure from molecular chains was not attempted, and is only briefly outlined here. The procedure described can be employed especially when standard crystallographic parameters are not available and traditional methods based on X-ray diffraction fail. Full article
(This article belongs to the Special Issue NMR Crystallography)
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15 pages, 7759 KiB  
Article
Determination of the Full 207Pb Chemical Shift Tensor of Anglesite, PbSO4, and Correlation of the Isotropic Shift to Lead–Oxygen Distance in Natural Minerals
by Otto E. O. Zeman, Jennifer Steinadler, Rupert Hochleitner and Thomas Bräuniger
Crystals 2019, 9(1), 43; https://doi.org/10.3390/cryst9010043 - 15 Jan 2019
Cited by 10 | Viewed by 4596
Abstract
The full 207 Pb chemical shift (CS) tensor of lead in the mineral anglesite, PbSO 4 , was determined from orientation-dependent nuclear magnetic resonance (NMR) spectra of a large natural single crystal, using a global fit over two rotation patterns. The resulting tensor [...] Read more.
The full 207 Pb chemical shift (CS) tensor of lead in the mineral anglesite, PbSO 4 , was determined from orientation-dependent nuclear magnetic resonance (NMR) spectra of a large natural single crystal, using a global fit over two rotation patterns. The resulting tensor is characterised by the reduced anisotropy Δ δ = ( − 327 ± 4 ) ppm, asymmetry η C S = 0.529 ± 0.002 , and δ i s o = ( − 3615 ± 3 ) ppm, with the isotropic chemical shift δ i s o also verified by magic-angle spinning NMR on a polycrystalline sample. The initially unknown orientation of the mounted single crystal was included in the global data fit as well, thus obtaining it from NMR data only. By use of internal crystal symmetries, the amount of data acquisition and processing for determination of the CS tensor and crystal orientation was reduced. Furthermore, a linear correlation between the 207 Pb isotropic chemical shift and the shortest Pb–O distance in the co-ordination sphere of Pb 2 + solely surrounded by oxygen has been established for a large database of lead-bearing natural minerals. Full article
(This article belongs to the Special Issue NMR Crystallography)
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13 pages, 2922 KiB  
Article
Cyclodextrin-Driven Formation of Double Six-Ring (D6R) Silicate Cage: NMR Spectroscopic Characterization from Solution to Crystals
by Mohamed Haouas, Clément Falaise, Charlotte Martineau-Corcos and Emmanuel Cadot
Crystals 2018, 8(12), 457; https://doi.org/10.3390/cryst8120457 - 7 Dec 2018
Cited by 8 | Viewed by 4256
Abstract
Identification and isolation of secondary building units (SBUs) from synthesis media of zeolites still represent a challenging task for chemists. The cage structure anion Si12O3012− known as the double six-ring (D6R) was synthesized from α-cyclodextrin (α-CD) mediated alkaline silicate [...] Read more.
Identification and isolation of secondary building units (SBUs) from synthesis media of zeolites still represent a challenging task for chemists. The cage structure anion Si12O3012− known as the double six-ring (D6R) was synthesized from α-cyclodextrin (α-CD) mediated alkaline silicate solutions and conditions of its stability and reactivity in aqueous solution were studied by using nuclear magnetic resonance (NMR) spectroscopy. A single crystal X-ray diffraction (XRD) analysis revealed a novel polymorph of the hybrid complex K12Si12O30·2α-CD·nD2O (n ≈ 30–40), which crystallizes in the orthorhombic C2221 space group symmetry with a = 14.841(4) Å, b = 25.855(6) Å, and c = 41.91(1) Å. The supramolecular adduct of the silicate anion sandwiched by two α-CDs forms a perfect symmetry matching the H-bonding donor-acceptor system between the organic macrocycle and the D6R unit. The driving force of such a hybrid assembly has found to be strongly dependent on the nature of the cation present as large alkali counter ions (K+, Rb+ and Cs+), which stabilize the D6R structure acting as templates. Lastly, we provided the first 29Si MAS NMR measurement of 3Q Si in an isolated D6R unit that allows the verification of the linear correlation between the chemical shift and <SiOSi> bond angle for 3Q Si species in DnR cages (n = 3, 4, 6). Full article
(This article belongs to the Special Issue NMR Crystallography)
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Graphical abstract

14 pages, 2116 KiB  
Article
NMR Crystallography of the Polymorphs of Metergoline
by Jiri Czernek, Martina Urbanova and Jiri Brus
Crystals 2018, 8(10), 378; https://doi.org/10.3390/cryst8100378 - 25 Sep 2018
Cited by 16 | Viewed by 4490
Abstract
Two polymorphs of the drug compound metergoline (C25H29N3O2) were investigated in detail by solid-state NMR measurements. The results have been analysed by an advanced procedure, which uses experimental input together with the results of quantum [...] Read more.
Two polymorphs of the drug compound metergoline (C25H29N3O2) were investigated in detail by solid-state NMR measurements. The results have been analysed by an advanced procedure, which uses experimental input together with the results of quantum chemical calculations that were performed for molecular crystals. In this way, it was possible to assign the total of 40 1H–13C correlation pairs in a highly complex system, namely, in the dynamically disordered polymorph with two independent molecules in the unit cell of a large volume of 4234 Å3. For the simpler polymorph, which exhibits only small-amplitude motions and has just one molecule in the unit cell with a volume of 529.0 Å3, the values of the principal elements of the 13C chemical shift tensors were measured. Additionally, for this polymorph, a set of crystal structure predictions were generated, and the {13C, 1H} isotropic and 13C anisotropic chemical shielding data were computed while using the gauge-including projector augmented-wave approach combined with the “revised Perdew-Burke-Ernzerhof“ exchange-correlation functional (GIPAW-RPBE). The experimental and theoretical results were combined in an application of the newly developed strategy to polymorph discrimination. This research thus opens up new routes towards more accurate characterization of the polymorphism of drug formulations. Full article
(This article belongs to the Special Issue NMR Crystallography)
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