Review
Chemistry, Physical
Sandeep Kumar Mishra, N. Suryaprakash
Summary: The splitting of signals in NMR spectrum is caused by the interaction of nuclear spins and the transmission of spin polarization through chemical bonds. The strength of interaction depends on the number of consecutive chemical bonds and molecular conformation. Analyzing the spectrum and determining coupling constants from complex 1H spectra remains challenging due to the small chemical shift dispersion. Various NMR experiments have been developed to accurately determine homo- and heteronuclear couplings while maintaining high resolution.
PROGRESS IN NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY
(2023)
Article
Biochemistry & Molecular Biology
Stephanie Watermann, Caroline Schmitt, Tobias Schneider, Thomas Hackl
Summary: H-1 NMR spectroscopy combined with chemometric methods was used to analyze the geographical origin of walnut samples. Different NMR spectra were compared for multivariate analysis and a support vector machine classifier was applied for sample differentiation. The study showed the potential of H-1-C-13 HSQC as a 2D NMR experiment for metabolomics studies.
Article
Chemistry, Multidisciplinary
Lixin Liang, Yi Ji, Zhenchao Zhao, Caitlin M. Quinn, Xiuwen Han, Xinhe Bao, Tatyana Polenova, Guangjin Hou
Summary: The phase modulated rotary resonance (PMRR) technique allows for the reintroduction of heteronuclear dipolar couplings while suppressing other interactions under a wide range of MAS conditions, with robust performance.
Article
Biophysics
Qi Xu, Jinze Li, Zhiqi Zhang, Qi Yang, Wei Zhang, Jia Yao, Yaxin Zhang, Yueye Zhang, Zhen Guo, Chao Li, Shuli Li, Changsong Zhang, Chuanxin Wang, Lutao Du, Chuanyu Li, Lianqun Zhou
Summary: Real-time digital polymerase chain reaction (qdPCR) integrates absolute quantification with process information, improving precision in molecular diagnostics. We propose a novel approach to determine optimal reaction conditions for qdPCR using real-time fluorescence monitoring in microwells. By leveraging an ultrathin laminated chip (UTL chip), we achieve faster amplification and higher accuracy, showing promise for molecular diagnostics.
BIOSENSORS & BIOELECTRONICS
(2024)
Article
Remote Sensing
Satoshi Ikari, Kyohei Akiyama, Yuki Igarashi, Kaori Kawate, Toshitaka Sasaki, Yasuyuki Watanabe, Takuji Ebinuma, Shinichi Nakasuka
Summary: We propose an accurate analytical non-gravitational force model of QZS-1, 2, and 4 for precise orbit determination. Using high-fidelity satellite geometry model and thermal information, we constructed detailed solar radiation pressure and thermal radiation pressure models. Based on the analytical model, we also proposed a hybrid model combined with the empirical approach. The results show that the proposed analytical model has better accuracy in orbit determination than the currently published orbit products obtained by empirical disturbance models.
Article
Chemistry, Physical
Junyan Wang, Feng An, Junjie Chen, Xixi Hu, Hua Guo, Daiqian Xie
Summary: A new and accurate diabatic potential energy matrix (DPEM) for the two lowest-lying electronic states of HO2 has been developed. The DPEM covers both the strong interaction region and reaction asymptotes. The accuracy of the electronic structure calculations is validated and the DPEM correctly predicts the properties of conical intersection seams, providing a reliable platform for studying spectroscopy and nonadiabatic dynamics of HO2.
JOURNAL OF CHEMICAL THEORY AND COMPUTATION
(2023)
Article
Materials Science, Multidisciplinary
Maral Sarebanzadeh, Alberto Orozco-Caballero, Javier LLorca
Summary: The transfer of basal-to-basal slip across grain boundaries was studied in weakly-textured pure Mg specimens deformed in tension using slip trace analysis and electron back-scatterer diffraction. Basal slip was the dominant deformation mechanism in most grains, and the transfer/blocking of slip at grain boundaries was examined. The active slip system(s) in the grains were determined by analyzing the rotation of grains caused by plastic slip along the basal slip systems. Additionally, the orientation of grain boundaries was measured to determine the twist angle theta.
Article
Spectroscopy
Xiaojuan Nie, Zhian Bao, Peng Liang, Kaiyun Chen, Chunlei Zong, Honglin Yuan
Summary: This study proposes a highly efficient method for direct determination of Zn isotopes in Zn-rich minerals using MC-ICP-MS without the need for column chromatography. The experimental results show that non-deviated Zn isotopic ratios can be obtained by correcting instrumental mass bias. The method demonstrates good long-term reproducibility and little drift in Zn isotopic ratios in Zn-rich minerals.
ATOMIC SPECTROSCOPY
(2022)
Article
Biochemical Research Methods
Marisa Maria, Nuno R. Neng, Thomas Berg
Summary: This study developed and validated an accurate and precise LC-MS/MS method for the determination of six PEth homologues in whole blood. The method is important for predicting different drinking patterns and has potential in assessing alcohol-related risks.
JOURNAL OF CHROMATOGRAPHY A
(2023)
Article
Chemistry, Analytical
Junichiro Ohta, Tatsuo Nozaki, Honami Sato, Kana Ashida, Yasuhiro Kato
Summary: The study presents a measurement procedure that minimizes contamination of osmium (Os) from external sources and enables accurate and precise measurements on small amounts of Os. The method utilizes a multiple collector-inductively coupled plasma-mass spectrometer equipped with compact discrete dynode (CDD) ion-counting detectors.
JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY
(2022)
Article
Orthopedics
Wazzan S. Aljuhani, Abdullah A. Alsaeed, Maali O. Alrashed, Abdullah M. Alanazi, Mohammed J. Alsalman
Summary: This study aimed to establish a quantitative and reproducible relationship between the position of the knee joint line and recognizable anatomical landmarks surrounding it. The lateral epicondyle to joint line distance was found to be a reliable landmark for accurate measurement of the knee joint line level.
JOURNAL OF EXPERIMENTAL ORTHOPAEDICS
(2023)
Article
Chemistry, Organic
Marketa Tichotova, Tomas Landovsky, Jan Lang, Sharon Jeziorowski, Volker Schmidts, Michal Kohout, Martin Babor, Pavel Lhotak, Christina M. Thiele, Hana Dvorakova
Summary: By using polyglutamates with different side-chain moieties (PBLG and PBPMLG) as alignment media, we achieved enantiodiscrimination of inherently chiral compounds for the first time. The experimental results not only provided more accurate structural information, but also revealed the conformational preferences and chiral alignment differences of phenoxathiin-based thiacalix[4]arenes in solution.
JOURNAL OF ORGANIC CHEMISTRY
(2023)
Article
Biochemical Research Methods
J. Kind, M. Stein, T. Gambaryan-Roisman, P. Stephan, T. L. Zankel, C. M. Thiele
Summary: Controlling and understanding the wetting and evaporation of complex fluids is crucial for improving processes like the production of organic semiconductors via printing. This study focuses on examining the time-dependent composition of complex fluid droplets during wetting or evaporation. The evaporation rate of water droplets depends on vapor pressures and humidity, thus it is necessary to measure and control humidity and temperature during measurements. By using MRI and spatially resolved NMR spectroscopy, the evaporation of droplets can be studied and compared with diffusive evaporation models and finite element numerical simulations. The findings reveal different evaporation regimes depending on flow rate and distance between gas outlet and droplet. The presented approach allows for comparative measurements and the observation of droplet evaporation in various environments. The setup can also control the evaporation rate of water from complex mixtures.
JOURNAL OF MAGNETIC RESONANCE
(2023)
Article
Chemistry, Multidisciplinary
Coral Mycroft, Guilherme Dal Poggetto, Thaiis M. Barbosa, Claiudio F. Tormena, Mathias Nilsson, Gareth A. Morris, Laura Castanar
Summary: The NMR analysis of fluorine-containing molecules is important in pharmaceuticals and biochemistry, but faces challenges due to severe peak overlap. This study introduces a new method, IPAP-FESTA, that simplifies measurements of proton-fluorine couplings. Its usefulness is demonstrated in the structural study of the drug fluticasone propionate and in assessing solvent effects on fluorohydrin conformational equilibrium in a mixture.
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY
(2023)
Article
Chemistry, Multidisciplinary
Johann J. Primozic, Julian Ilgen, Patrick Maibach, Matthias Brauser, Jonas Kind, Christina M. Thiele
Summary: The Pd-catalyzed allylic alkylation of 3,4-disubstituted, racemic cyclobutene electrophiles shows an unusual stereoselectivity. Stereoinduction is controlled by the choice of ligand and is independent of the substrate's configuration. Mechanistic investigations reveal deviations from the commonly accepted double inversion rule and the formation of unreactive syn-Pd-cyclobutene complexes due to strong internal Pd-O chelation.
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY
(2023)
Article
Chemistry, Multidisciplinary
Coral Mycroft, Marshall J. Smith, Mathias Nilsson, Gareth A. Morris, Laura Castanar
Summary: NMR measurements of molecules with sparse fluorine atoms are common in medicinal chemistry, but are complicated by homonuclear and heteronuclear scalar couplings. FESTA, a heteronuclear spectral editing method, simplifies 1H NMR spectra by obtaining only H-1 signals from the same spin system as a chosen F-19. However, signal overlap due to scalar couplings remains a problem in FESTA spectra.
MAGNETIC RESONANCE IN CHEMISTRY
(2023)
Article
Chemistry, Multidisciplinary
Marshall J. Smith, Jack E. Bramham, Mathias Nilsson, Gareth A. Morris, Laura Castanar, Alexander P. Golovanov
Summary: Fluorine is widely used in medicinal chemistry, both in drug molecules and molecular probes, due to its convenient monitoring capabilities by NMR spectroscopy in complex environments. However, NMR sensitivity is limited, especially at low concentrations of molecules.
CHEMICAL COMMUNICATIONS
(2023)
Article
Chemistry, Multidisciplinary
Daniel A. Taylor, Peter Kiraly, Paul Bowyer, Mathias Nilsson, Laura Castanar, Gareth A. Morris, Ralph W. Adams
Summary: Selective 1D COSY can identify coupled spins but has limitations in selectivity and multiplet lineshapes. This study combines ultra-selective GEMSTONE excitation with CLIP-COSY to provide through-bond correlations for overlapping NMR signals. The method is demonstrated using the drugs lasalocid and cyclosporin.
CHEMICAL COMMUNICATIONS
(2023)
Article
Chemistry, Organic
Marshall J. J. Smith, Emma L. L. Gates, Goran Widmalm, Ralph W. W. Adams, Gareth A. A. Morris, Mathias Nilsson
Summary: Human milk oligosaccharides are bioactive molecules that have diverse effects on infant development. NMR provides important structural information about these oligosaccharides, but signal overlap in the spectra makes this information difficult to obtain. This study demonstrates the benefits of combining pure shift methods with the CASPER computational approach for resonance assignment in oligosaccharides.
ORGANIC & BIOMOLECULAR CHEMISTRY
(2023)
Article
Chemistry, Multidisciplinary
Max Hirschmann, Olaf Soltwedel, Philipp Ritzert, Regine von Klitzing, Christina M. Thiele
Summary: Two polyaspartates with ortho-fluorinated azo-benzenes (pFAB) as photo-responsive groups in the side chain were synthesized: PpFABLA (1) and co-polyaspartate PpFABLA-co-PBLA [11, 75%(n/n) PpFABLA content]. PpFABLA (1) undergoes a visible-light-induced reversible coil-helix transition in solution due to the E/Z-isomerization of the side chain. PpFABLA-co-PBLA (11) forms a helix independently of the E/Z-isomerization of the side chain and exhibits changes in the morphology and dipolar coupling.
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY
(2023)
Article
Chemistry, Multidisciplinary
Elsa Caytan, Howard M. Foster, Laura Castanar, Ralph W. Adams, Mathias Nilsson, Gareth A. Morris
Summary: This study reveals that practical pure shift NMR experiments using cryoprobes may result in signal loss, and proposes a simple adjustment to recover the lost signal.
CHEMICAL COMMUNICATIONS
(2023)
Review
Chemistry, Multidisciplinary
Dan He, Yawen Li, Fuwen Zhao, Yuze Lin
Summary: High trap density in organic solar cells leads to localized charge carriers and reduced carrier lifetime, limiting device efficiency. This feature article summarizes the recent advances of trap suppression by material design and device engineering.
CHEMICAL COMMUNICATIONS
(2024)
Review
Chemistry, Multidisciplinary
Olivier Monfort, Arshitha Madhusudhan, Martin Motola
Summary: This article presents the advantages of coupling photocatalysis and Fenton-based processes for environmental remediation and discusses their synergy. It critically examines the simultaneous triggering of these two processes and provides insights into research approaches. The study aims to enhance understanding of this complex process and highlight the potential integration of new catalysts in current wastewater treatment technology.
CHEMICAL COMMUNICATIONS
(2024)
Article
Chemistry, Multidisciplinary
Manideepa Dhar, Chittaranjan Mishra, Avijit Das, Uttam Manna
Summary: An approach of 'polymerization of monomers in its aggregated form' has been introduced to tailor the water wettability of fibrous and porous substrates, achieving hydrophobicity to superhydrophobicity transition, as well as patterned wettability. This facile chemical method provides a durable coating with adjustable and patterned wettability for various potential applications.
CHEMICAL COMMUNICATIONS
(2024)
Article
Chemistry, Multidisciplinary
Saswat Ranjan Bhoi, Chhanda Debnath, Shikha Gandhi
Summary: In this article, a novel catalytic reaction using Pd(0) and Bronsted acid is reported for the synthesis of biologically important imidazolidinone-fused N-heterocycles through redox-neutral intramolecular N-allylation of indoles and pyrroles with alkynes. This atom-economical method is applicable to a wide range of substrates and eliminates the need for leaving groups or oxidizing agents commonly used in traditional allylation reactions.
CHEMICAL COMMUNICATIONS
(2024)
Article
Chemistry, Multidisciplinary
Longkun Chen, Mingshuai Zhang, Meichen Liu, Zhuoyuan Liu, Yuetong Qiu, Zhilai Zhang, Fuchao Yu, Jiuzhong Huang
Summary: In this study, an efficient Rh(III)-catalyzed selective mono- and dual-C-H bond functionalization/cyclization with iodonium ylide as the sole coupling partner was demonstrated. Fused benzodiazepine skeletons were obtained in excellent yields, providing an improved approach to dual C-H unsymmetrical functionalization.
CHEMICAL COMMUNICATIONS
(2024)
Article
Chemistry, Multidisciplinary
Alice Kennett, Sven Epple, Gabriella van der Valk, Irene Georgiou, Evelyne Gout, Romain R. Vives, Angela J. Russell
Summary: This study presents the design and synthesis of sulfated disaccharide inhibitors based on IdoA(2S)-GlcNS(6S), which showed potent inhibition of Sulf-2. The results suggest that IdoA(2S)-GlcNS(6S) is the shortest fragment size required for effective inhibition of Sulfs, and a trisulfated disaccharide is identified as the minimal fragment size of heparan sulfate for effective endosulfatase inhibition.
CHEMICAL COMMUNICATIONS
(2024)
Article
Chemistry, Multidisciplinary
Mauro Garbini, Andrea Brunetti, Riccardo Pedrazzani, Magda Monari, Massimo Marcaccio, Giulio Bertuzzi, Marco Bandini
Summary: The self-adaptability of galvanostatic electrolysis was found to be helpful in a multistage chemo- and diastereoselective electrochemically promoted cyclodimerization of chalcones. Through a series of reductive events, densely functionalized cyclopentanes with five contiguous stereocenters were obtained (25 examples, yields up to 95%, dr values up to >20:1). Further experimental and electrochemical investigations indicated the crucial role of dynamic kinetic resolution of the aldol intermediate in the reaction mechanism.
CHEMICAL COMMUNICATIONS
(2024)
Article
Chemistry, Multidisciplinary
Dhananjay S. Nipate, Neha Meena, Prakash N. Swami, Krishnan Rangan, Anil Kumar
Summary: In this study, the synthesis of functionalized benzo[a]phenazines and indazolo[2,3-a]quinolines was achieved through Rh(III)-catalyzed oxidative annulation of 2-arylquinoxalines and 2-aryl-2H-indazoles with allyl alcohols. The method showed a wide substrate scope, excellent functional group tolerance, good to high yields of annulated products, and the capability for scaled-up synthesis. A tentative mechanism of the annulation reaction was proposed based on a preliminary mechanistic investigation.
CHEMICAL COMMUNICATIONS
(2024)
Article
Chemistry, Multidisciplinary
Ruonan Zhang, Abudukadi Tudi, Xia Yang, Xuping Wang, Zhihua Yang, Shujuan Han, Shilie Pan
Summary: A new lead tellurium borate material with a unique fundamental building block [B4O10] was synthesized and found to exhibit high birefringence. The structure-property relationship was discussed using first-principles calculations.
CHEMICAL COMMUNICATIONS
(2024)
Article
Chemistry, Multidisciplinary
Amresh Kumar Singh, Baishali Thakurta, Anupam Giri, Monalisa Pal
Summary: This study introduces three key concepts for the quick synthesis of large-scale high-quality 2D materials films and their utilization in device fabrication.
CHEMICAL COMMUNICATIONS
(2024)
Article
Chemistry, Multidisciplinary
Reina Hagiwara, Shun Nishimura, Kosuke Okeyoshi
Summary: A copolymer-conjugated nanocatalytic system has been developed to improve electron transfer and enhance photoinduced H2 generation.
CHEMICAL COMMUNICATIONS
(2024)
