scholarly journals Hydrogen-Mediated Noncovalent Interactions in Solids: What Can NMR Crystallography Tell About?

Molecules ◽  
2020 ◽  
Vol 25 (16) ◽  
pp. 3757
Author(s):  
Ioana Georgeta Grosu ◽  
Xenia Filip ◽  
Maria O. Miclăuș ◽  
Claudiu Filip
Keyword(s):  
Crystal Engineering ◽  
Rational Design ◽  
Noncovalent Interactions ◽  
Molecular Crystals ◽  
Labile Hydrogen ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Practical Applications ◽  
Comprehensive Picture ◽  
Nmr Crystallography

Hydrogen atoms play a crucial role in the aggregation of organic (bio)molecules through diverse number of noncovalent interactions that they mediate, such as electrostatic in proton transfer systems, hydrogen bonding, and CH–π interactions, to mention only the most prominent. To identify and adequately describe such low-energy interactions, increasingly sensitive methods have been developed over time, among which quantum chemical computations have witnessed impressive advances in recent years. For reaching the present state-of-the-art, computations had to rely on a pool of relevant experimental data, needed at least for validation, if not also for other purposes. In the case of molecular crystals, the best illustration for the synergy between computations and experiment is given by the so-called NMR crystallography approach. Originally designed to increase the confidence level in crystal structure determination of organic compounds from powders, NMR crystallography is able now to offer also a wealth of information regarding the noncovalent interactions that drive molecules to pack in a given crystalline pattern or another. This is particularly true for the noncovalent interactions which depend on the exact location of labile hydrogen atoms in the system: in such cases, NMR crystallography represents a valuable characterization tool, in some cases complementing even the standard single-crystal X-ray diffraction technique. A concise introduction in the field is made in this mini-review, which is aimed at providing a comprehensive picture with respect to the current accuracy level reached by NMR crystallography in the characterization of hydrogen-mediated noncovalent interactions in organic solids. Different types of practical applications are illustrated with the example of molecular crystals studied by our research group, but references to other representative developments reported in the literature are also made. By summarizing the major concepts and methodological progresses, the present work is also intended to be a guide to the practical potential of this relatively recent analytical tool for the scientists working in areas where crystal engineering represents the main approach for rational design of novel materials.

FACILE SYNTHESIS OF HYDROXYLAPATITE NANOSTRUCTURES WITH VARIOUS MORPHOLOGIES

NANO ◽  
2009 ◽  
Vol 04 (03) ◽  
pp. 165-170 ◽  
Author(s):  
XIAO-JUN HU ◽  
JIN-KU LIU ◽  
XIAO-YAN QIN ◽  
JIA HUANG ◽  
YI YI
Keyword(s):  
Crystal Engineering ◽  
Fourier Transforms ◽  
X Ray Diffraction ◽  
X Ray ◽  
Solution Approach ◽  
Engineering Research ◽  
Practical Applications ◽  
Transmission Electron ◽  
Ft Ir ◽  
Fourier Transforms Infrared Spectroscopy

The hydroxylapatite nanostructures with different morphologies have been synthesized by a facile solution approach. The samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) technologies, and Fourier transforms infrared spectroscopy (FT-IR). The control mechanism of the hydroxylapatite with various morphologies nanostructures was investigated. Some practical experimental conclusions could be obtained, which were expected to have potential values in crystal engineering research and practical applications.

scholarly journals Structural Refinement of Carbimazole by NMR Crystallography

Molecules ◽  
2021 ◽  
Vol 26 (15) ◽  
pp. 4577
Author(s):  
Andrea Scarperi ◽  
Giovanni Barcaro ◽  
Aleksandra Pajzderska ◽  
Francesca Martini ◽  
Elisa Carignani ◽  
...  
Keyword(s):  
Diffraction Data ◽  
Geometry Optimization ◽  
Optimization Methods ◽  
2D Nmr ◽  
Dimensional Structure ◽  
Structural Refinement ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
X Ray ◽  
Nmr Crystallography

The characterization of the three-dimensional structure of solids is of major importance, especially in the pharmaceutical field. In the present work, NMR crystallography methods are applied with the aim to refine the crystal structure of carbimazole, an active pharmaceutical ingredient used for the treatment of hyperthyroidism and Grave’s disease. Starting from previously reported X-ray diffraction data, two refined structures were obtained by geometry optimization methods. Experimental 1H and 13C isotropic chemical shift measured by the suitable 1H and 13C high-resolution solid state NMR techniques were compared with DFT-GIPAW calculated values, allowing the quality of the obtained structure to be experimentally checked. The refined structure was further validated through the analysis of 1H-1H and 1H-13C 2D NMR correlation experiments. The final structure differs from that previously obtained from X-ray diffraction data mostly for the position of hydrogen atoms.

scholarly journals Flux Method Growth of Large Size Group IV–V 2D GeP Single Crystals and Photoresponse Application

Crystals ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 235
Author(s):  
Shuqi Zhao ◽  
Tongtong Yu ◽  
Ziming Wang ◽  
Shilei Wang ◽  
Limei Wei ◽  
...  
Keyword(s):  
Raman Spectroscopy ◽  
Single Crystals ◽  
High Performance ◽  
Group Iv ◽  
X Ray Diffraction ◽  
High Quality ◽  
Practical Applications ◽  
Large Size ◽  
Growth Method ◽  
Polarized Raman

Two-dimensional (2D) materials driven by their unique electronic and optoelectronic properties have opened up possibilities for their various applications. The large and high-quality single crystals are essential to fabricate high-performance 2D devices for practical applications. Herein, IV-V 2D GeP single crystals with high-quality and large size of 20 × 15 × 5 mm3 were successfully grown by the Bi flux growth method. The crystalline quality of GeP was confirmed by high-resolution X-ray diffraction (HRXRD), Laue diffraction, electron probe microanalysis (EPMA) and Raman spectroscopy. Additionally, intrinsic anisotropic optical properties were investigated by angle-resolved polarized Raman spectroscopy (ARPRS) and transmission spectra in detail. Furthermore, we fabricated high-performance photodetectors based on GeP, presenting a relatively large photocurrent over 3 mA. More generally, our results will significantly contribute the GeP crystal to the wide optoelectronic applications.

Theoretically derived thermodynamic properties can be improved by the refinement of low-frequency modes against X-ray diffraction data

2021 ◽  
Author(s):  
Anna Agnieszka Hoser ◽  
Marcin Sztylko ◽  
Damian Trzybiński ◽  
Anders Østergaard Madsen
Keyword(s):  
Thermodynamic Properties ◽  
Dft Calculations ◽  
Diffraction Data ◽  
Molecular Crystals ◽  
Low Frequency ◽  
X Ray Diffraction ◽  
X Ray ◽  
Efficient Approach

A framework for estimation of thermodynamic properties for molecular crystals via refinement of frequencies from DFT calculations against X-ray diffraction data is presented. The framework provides an efficient approach to...

In situ nanoscale visualization of solvent effects on molecular crystal surfaces

CrystEngComm ◽  
2021 ◽  
Author(s):  
Mikkel Herzberg ◽  
Anders Støttrup Larsen ◽  
Tue Hassenkam ◽  
Anders Østergaard Madsen ◽  
Jukka Rantanen
Keyword(s):  
Solid Solution ◽  
Solvent Effects ◽  
Molecular Crystal ◽  
Rational Design ◽  
Molecular Level ◽  
Molecular Crystals ◽  
Crystal Surfaces ◽  
Solution Interface ◽  
Atomic Force

Solvents can dramatically affect molecular crystals. Obtaining favorable properties for these crystals requires rational design based on molecular level understanding of the solid-solution interface. Here we show how atomic force...

scholarly journals Engineering Ruthenium-Based Electrocatalysts for Effective Hydrogen Evolution Reaction

2021 ◽  
Vol 13 (1) ◽  
Author(s):  
Yingjie Yang ◽  
Yanhui Yu ◽  
Jing Li ◽  
Qingrong Chen ◽  
Yanlian Du ◽  
...  
Keyword(s):  
Hydrogen Evolution ◽  
Hydrogen Evolution Reaction ◽  
Rational Design ◽  
Energy System ◽  
Structure Design ◽  
Single Atom ◽  
Research Progress ◽  
Pure Hydrogen ◽  
Hydrogen Energy ◽  
Practical Applications

AbstractThe investigation of highly effective, durable, and cost-effective electrocatalysts for the hydrogen evolution reaction (HER) is a prerequisite for the upcoming hydrogen energy society. To establish a new hydrogen energy system and gradually replace the traditional fossil-based energy, electrochemical water-splitting is considered the most promising, environmentally friendly, and efficient way to produce pure hydrogen. Compared with the commonly used platinum (Pt)-based catalysts, ruthenium (Ru) is expected to be a good alternative because of its similar hydrogen bonding energy, lower water decomposition barrier, and considerably lower price. Analyzing and revealing the HER mechanisms, as well as identifying a rational design of Ru-based HER catalysts with desirable activity and stability is indispensable. In this review, the research progress on HER electrocatalysts and the relevant describing parameters for HER performance are briefly introduced. Moreover, four major strategies to improve the performance of Ru-based electrocatalysts, including electronic effect modulation, support engineering, structure design, and maximum utilization (single atom) are discussed. Finally, the challenges, solutions and prospects are highlighted to prompt the practical applications of Ru-based electrocatalysts for HER.

SYNTHESIS OF NEW 1223-TYPE LAYERED CUPRATE (Tl, V) (Sr, Ba)2Ca2Cu3O9 WITH TC(ρ=0) ABOVE 110 K

1993 ◽  
Vol 07 (11) ◽  
pp. 761-769 ◽  
Author(s):  
Z.Y. CHEN ◽  
Z.Z. SHENG ◽  
Y.F. LI ◽  
D.O. PEDERSON
Keyword(s):  
X Ray Diffraction ◽  
X Ray ◽  
Practical Applications ◽  
Layered Cuprates

A new series of 1223-type (Tl, V)-based layered cuprates (Tl, V)(Sr,Ba) 2 Ca 2 Cu 3 O 9 has been successfully synthesized and identified by powder X-ray diffraction. Partial substitutions of V for Tl and Ba for Sr promote the formation of (Tl, V)-based 1223-type compounds. Nominal samples ( Tl 1−x V x) ( Sr 2−y Ba y) Ca 2 Cu 3 O z with x=0.25–0.50 and y=0.25–1.50 are pure or nearly-pure 1223 phase and exhibit TC(ρ=0) in the range of 100–110 K. This new (Tl, V)-based high TC material may be of importance in practical applications.

The first proof of protonated anion tetrahedra in the tsumcorite-type compounds

2004 ◽  
Vol 68 (5) ◽  
pp. 757-767 ◽  
Author(s):  
T. Mihajlović ◽  
H. Effenberger
Keyword(s):  
Crystal Structure ◽  
Hydrothermal Synthesis ◽  
Single Crystal ◽  
Diffraction Data ◽  
Title Compound ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
Synthetic Compounds ◽  
X Ray

AbstractHydrothermal synthesis produced the new compound SrCo2(AsO4)(AsO3OH)(OH)(H2O). The compound belongs to the tsumcorite group (natural and synthetic compounds with the general formula M(1)M(2)2(XO4)2(H2O,OH)2; M(1)1+,2+,3+ = Na, K, Rb, Ag, NH4, Ca, Pb, Bi, Tl; M(2)2+,3+ = Al, Mn3+, Fe3+, Co, Ni, Cu, Zn; and X5+,6+ = P, As, V, S, Se, Mo). It represents (1) the first Sr member, (2) the until now unknown [7]-coordination for the M(1) position, (3) the first proof of (partially) protonated arsenate groups in this group of compounds, and (4) a new structure variant.The crystal structure of the title compound was determined using single-crystal X-ray diffraction data. The compound is monoclinic, space group P21/a, with a = 9.139(2), b = 12.829(3), c = 7.522(2) Å, β = 114.33(3)°, V = 803.6(3) Å3, Z = 4 [wR2 = 0.065 for 3530 unique reflections]. The hydrogen atoms were located experimentally.

scholarly journals Hydrogen atoms in protein structures: high-resolution X-ray diffraction structure of the DFPase

2013 ◽  
Vol 6 (1) ◽  
pp. 308 ◽  
Author(s):  
Mikael Elias ◽  
Dorothee Liebschner ◽  
Jurgen Koepke ◽  
Claude Lecomte ◽  
Benoit Guillot ◽  
...  
Keyword(s):  
High Resolution ◽  
Protein Structures ◽  
X Ray Diffraction ◽  
Hydrogen Atoms ◽  
X Ray ◽  
Diffraction Structure
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