Philipp Willmer, Adam C. Hundahl, Rodolphe Marie, Henrik Jensen
{"title":"Cover Picture: Continuous Titration Based Method for Rapid In-Solution Analysis of Non-Covalent Interactions (Chem. Methods 5/2025)","authors":"Philipp Willmer, Adam C. Hundahl, Rodolphe Marie, Henrik Jensen","doi":"10.1002/cmtd.202580501","DOIUrl":"https://doi.org/10.1002/cmtd.202580501","url":null,"abstract":"<p><b>The Front Cover</b> illustrates a new method (cSPRING) to study the interaction of a target molecule exposed to a continuous titration of a small ligand inside a flow capillary. The fluorescence emission of the target is detected in two separate spectral bands. A ratiometric measurement allows to extract the binding affinity (<i>K</i><i><sub>d</sub></i>) from a single measurement. Requiring only two samples and less than a minute, this method is well-suited for high-throughput screening applications. For more details, see the Research Article by Henrik Jensen and co-workers (10.1002/cmtd.202400059).\u0000 <figure>\u0000 <div><picture>\u0000 <source></source></picture><p></p>\u0000 </div>\u0000 </figure>\u0000 </p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"5 5","pages":""},"PeriodicalIF":6.1,"publicationDate":"2025-05-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202580501","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143944423","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
José Nuno Almeida, Lu Song, Sohrab Askarli, Sang-Ho Chung, Javier Ruiz-Martínez
{"title":"Cover Picture: Zeolite–Water Chemistry: Characterization Methods to Unveil Zeolite Structure (Chem. Methods 4/2025)","authors":"José Nuno Almeida, Lu Song, Sohrab Askarli, Sang-Ho Chung, Javier Ruiz-Martínez","doi":"10.1002/cmtd.202580401","DOIUrl":"https://doi.org/10.1002/cmtd.202580401","url":null,"abstract":"<p><b>The Front Cover</b> illustrates a zeolite framework enclosed within a protective dome, symbolizing its characterization under water-free conditions. This review explores the impact of water on zeolite structure, acidity, and stability. It highlights advanced in-situ NMR and FTIR techniques for probing how water interacts with active sites, along with complementary dehydration strategies to remove water from zeolites. By refining zeolite characterization, this study offers valuable insights into optimizing their catalytic performance. For more details, see the Review Article by Sang-Ho Chung, Javier Ruiz-Martínez, and co-workers (DOI: 10.1002/cmtd.202400076).\u0000 <figure>\u0000 <div><picture>\u0000 <source></source></picture><p></p>\u0000 </div>\u0000 </figure>\u0000 </p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"5 4","pages":""},"PeriodicalIF":6.1,"publicationDate":"2025-04-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202580401","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143793311","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
José Nuno Almeida, Lu Song, Sohrab Askarli, Sang-Ho Chung, Javier Ruiz-Martínez
{"title":"Zeolite–Water Chemistry: Characterization Methods to Unveil Zeolite Structure","authors":"José Nuno Almeida, Lu Song, Sohrab Askarli, Sang-Ho Chung, Javier Ruiz-Martínez","doi":"10.1002/cmtd.202400076","DOIUrl":"https://doi.org/10.1002/cmtd.202400076","url":null,"abstract":"<p>This review provides comprehensive aspects of the interaction of water with zeolites, focusing on its influence on the structural and catalytic properties of zeolites. It details how water can alter zeolite acidity by forming hydrogen bonding or hydronium ions through different modes of water in zeolite topologies. Moreover, it summarizes the risks of zeolite stability loss <i>via</i> hydrolysis of Si−O−T bonds to influence the stability, structure, and catalytic reactivity of zeolites. To address water interference, various strategies for water removal from zeolite frameworks are reviewed and proposed from the structural perspective of the zeolites. By combining advanced <i>in-situ</i> techniques, FTIR and solid-state NMR have proven effective in providing atomic-level insights, as they eliminate the masking effects of water to enable precise characterization of the zeolite framework. This work underscores the importance of these methods in minimizing the influence of water, enhancing the reliability of zeolite characterization for catalytic applications, and providing insights into recent advancements, challenges, and future directions in the related fields.</p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"5 4","pages":""},"PeriodicalIF":6.1,"publicationDate":"2025-03-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202400076","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143793347","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Abdul Mannan Butt, Abhijit Nag, Praveen B. Managutti, Sharmarke Mohamed, Faisal AlMarzooqi, Ahsanulhaq Qurashi
{"title":"Method-Induced Isomerism and Concentration Mediated Isolation of Two (Cu14 and Cu41) Atomically Precise Copper Nanoclusters","authors":"Abdul Mannan Butt, Abhijit Nag, Praveen B. Managutti, Sharmarke Mohamed, Faisal AlMarzooqi, Ahsanulhaq Qurashi","doi":"10.1002/cmtd.202400031","DOIUrl":"https://doi.org/10.1002/cmtd.202400031","url":null,"abstract":"<p>Ligand-protected atomically precise metal nanoclusters (MNCs) have attracted peculiar interest not only for their distinct molecular structure but also for their unique physiochemical properties, providing an ideal platform for developing structure-activity correlation at the atomic level. In this work, we have presented the isolation of two nanoclusters (NCs) [Cu<sub>14</sub>H<sub>10</sub>(DMBT)<sub>3</sub>(PPh<sub>3</sub>)<sub>8</sub>][BF<sub>4</sub>] (<b>Cu<sub>14</sub></b>) and [Cu<sub>41</sub>H<sub>21</sub>Cl<sub>8</sub>(DMBT)<sub>12</sub>(PPh<sub>3</sub>)<sub>6</sub>] (<b>Cu<sub>41</sub></b>) [DMBT=2,4-dimethylbenzenethiol and PPh<sub>3</sub>=Triphenylphosphine] upon manipulating the concentration of thiol ligand. A correlation between thiolate ligand's concentration and product selectivity was noticed. Further, the presence of R and S isomerism was observed in Cu<sub>14</sub> unit cell. Single Crystal X-ray Diffraction (SC-XRD) data revealed that Cu<sub>14</sub> crystallized in the cubic space group <i>Pa</i>-3, while Cu<sub>41</sub> in hexagonal space group <i>P</i>6<sub>3</sub>/<i>m</i>. The crystal structure of Cu<sub>14</sub> and Cu<sub>41</sub> NCs were supported using high resolution electrospray mass spectrometry (ESI MS) and other spectroscopic approaches. We believe this study will serve as a guide for controllable synthesis of MNCs.</p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"5 4","pages":""},"PeriodicalIF":6.1,"publicationDate":"2025-03-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202400031","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143793809","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Dr. Elizaveta A. Fedorova, Dr. Aleksandr Fedorov, Dr. Dmitry E. Doronkin, Dr. David Linke, Dr. Christoph Kubis, Prof. Dr. Angelika Brückner, Prof. Dr. Evgenii V. Kondratenko
{"title":"Revealing the Mechanism and Kinetics of Fe5C2 Formation From Ferrous Oxalate under CO2 Fischer-Tropsch Conditions Using Time-Resolved In Situ X-Ray Absorption Spectroscopy","authors":"Dr. Elizaveta A. Fedorova, Dr. Aleksandr Fedorov, Dr. Dmitry E. Doronkin, Dr. David Linke, Dr. Christoph Kubis, Prof. Dr. Angelika Brückner, Prof. Dr. Evgenii V. Kondratenko","doi":"10.1002/cmtd.202400058","DOIUrl":"https://doi.org/10.1002/cmtd.202400058","url":null,"abstract":"<p>The fundamentals of in situ formation of iron carbides are required for the tailored design of Fe-based catalysts for the efficient conversion of CO<sub>2</sub> to higher hydrocarbons. Herein, time-resolved in situ X-ray absorption spectroscopy has been used to elucidate the mechanism of the formation of Fe<sub>5</sub>C<sub>2</sub> from ferrous oxalate (FeC<sub>2</sub>O<sub>4</sub>) at 350 °C using a H<sub>2</sub>/CO=3 reaction feed. Regardless of the kind of alkali metal promoter and reaction pressure (1 or 7.5 bar), FeC<sub>2</sub>O<sub>4</sub> is first decomposed to FeO followed by the conversion of the latter to Fe<sub>5</sub>C<sub>2</sub>. Further insights into the above transformations were derived by kinetic analysis using a Johnson–Mehl–Avrami–Erofeev–Kolmogorov model and kinetics-constrained neural ordinary differential equations method. Both approaches revealed that the formation of FeO at 1 bar follows a nucleation mechanism, while a diffusion mechanism has a higher contribution at 7.5 bar. The latter mechanism is valid for the conversion of FeO to Fe<sub>5</sub>C<sub>2</sub> at both pressures. Alkali metal promoters were found to accelerate the rate of Fe<sub>5</sub>C<sub>2</sub> formation. This rate decreases with increasing total pressure due to the stabilization of FeO.</p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"5 5","pages":""},"PeriodicalIF":6.1,"publicationDate":"2025-03-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202400058","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143944820","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Dr. Katarzyna Dziubińska-Kühn, Dr. Guzel Musabirova, Sophie Effertz, Prof. Jörg Matysik, Prof. Renaud Blaise Jolivet
{"title":"Cover Picture: Sodium-Potassium Competition as a Tool for Chemoselective Cucurbit[n]uril-Xenon Host–Guest Complexation in Imaging Applications (Chem. Methods 3/2025)","authors":"Dr. Katarzyna Dziubińska-Kühn, Dr. Guzel Musabirova, Sophie Effertz, Prof. Jörg Matysik, Prof. Renaud Blaise Jolivet","doi":"10.1002/cmtd.202580301","DOIUrl":"https://doi.org/10.1002/cmtd.202580301","url":null,"abstract":"<p><b>The Front Cover</b> illustrates that by paw-holding, wild sea otters ensure they stay together and do not drift apart in their sleep. This comes from a concept of no herd member being left behind. If the experimental conditions are met, the same phenomenon is observed in the study by Renaud Blaise Jolivet and co-workers, where K<sup>+</sup> ions and cage molecules interact in the solution, forming species with significantly higher Xe encapsulation rates. The preferential caging of Xe by CB[6]-alkali pairs is seen as an analogy to the paw-holding-based social gathering of sea otters. For more details, see the Research Article by Renaud Blaise Jolivet and co-workers (DOI: 10.1002/cmtd.202400033).\u0000 <figure>\u0000 <div><picture>\u0000 <source></source></picture><p></p>\u0000 </div>\u0000 </figure>\u0000 </p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"5 3","pages":""},"PeriodicalIF":6.1,"publicationDate":"2025-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202580301","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143581788","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Integrating Flow Chemistry With Electrospray Ionization Mass Spectrometry","authors":"Quentin Duez","doi":"10.1002/cmtd.202400036","DOIUrl":"https://doi.org/10.1002/cmtd.202400036","url":null,"abstract":"<p>Flow chemistry is a transformative method that facilitates the exploration of chemical reactivity and enables process automation. In this context of high-throughput experimentation, analysing reaction outputs often constitutes a bottleneck. The direct integration of flow chemistry with electrospray ionization mass spectrometry (ESI-MS) is emerging as a method for the real-time monitoring of reaction mixtures in flow conditions, paving the way for reaction optimization and mechanistic investigations. As shown in selected examples, flow chemistry coupled to ESI-MS facilitates the detection and characterization of reaction intermediates and allows for tracking reaction dynamics under continuously changing conditions. Furthermore, establishing direct feedback between the flow setup and the analytical instrument enables the autonomous optimization of experimental conditions based on the real-time MS readout. Altogether, MS approaches hold the potential to streamline the development of complex synthetic pathways in flow.</p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"5 4","pages":""},"PeriodicalIF":6.1,"publicationDate":"2025-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202400036","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143793436","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Vitaly P. Kozinenko, Alexey S. Kiryutin, Alexandra V. Yurkovskaya
{"title":"SLIC-SABRE at Microtesla Fields Enables High Levels of Nuclear Spin Polarization Without Magnetic Shielding","authors":"Vitaly P. Kozinenko, Alexey S. Kiryutin, Alexandra V. Yurkovskaya","doi":"10.1002/cmtd.202400060","DOIUrl":"https://doi.org/10.1002/cmtd.202400060","url":null,"abstract":"<p>Employing nuclear spin hyperpolarization to enhance NMR sensitivity opens new horizons for metabolic studies and chemical reaction monitoring. Among the hyperpolarization techniques, Signal Amplification by Reversible Exchange (SABRE) is prominent for its ability to transfer spin order from parahydrogen to target nuclei, especially <sup>13</sup>C and <sup>15</sup>N, without the chemical modification of the substrate under study. Despite its power, existing implementations of SABRE require expensive equipment like radiofrequency (RF) hardware and magnetic shielding. This paper demonstrates the SLIC-SABRE (Spin Lock Induced Crossing SABRE) method at low magnetic fields as a low-cost and efficient technique for achieving high <sup>15</sup>N polarization using a simple setup, consisting only of a small set of magnetic coils driven by a desktop PC sound card. The method yields from 5 up to 17 % polarization across various SABRE-active molecules, outperforming the conventional SABRE-SHEATH (SABRE in SHield Enables Alignment Transfer to Heteronuclei) approach and significantly enhancing the accessibility of hyperpolarization techniques.</p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"5 5","pages":""},"PeriodicalIF":6.1,"publicationDate":"2025-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202400060","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143944961","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Dr. Qing Wu, Han Zhou, Prof. Loïc Bertrand, Prof. Maartje Stols-Witlox, Prof. Laura Brambilla, Prof. Edith Joseph
{"title":"Natural and Artificial Aging Methods For Silver Mock-ups In Recent Conservation And Heritage Studies: A Short Review","authors":"Dr. Qing Wu, Han Zhou, Prof. Loïc Bertrand, Prof. Maartje Stols-Witlox, Prof. Laura Brambilla, Prof. Edith Joseph","doi":"10.1002/cmtd.202400055","DOIUrl":"https://doi.org/10.1002/cmtd.202400055","url":null,"abstract":"<p>Silver has been widely used for art and heritage objects throughout history, due to its excellent ductility, malleability and brilliant metallic lustre. However, silver objects tarnish over time and must be regularly treated to maintain their appearance. In conservation and heritage studies, naturally or artificially aged silver mock-ups are often used to simulate the tarnishing conditions of valuable historical silver objects. Over the last few decades, many research groups have proposed different aging protocols. In this paper, we reviewed the silver aging protocols employed in recent studies in the field. Although the chemistry-based aging methods are most widely used, issues regarding alterations of the tarnish stratigraphy and negative influences on environment and operator safety should not be neglected. This review aims to provide important references for conservators, scientists and researchers to select safe and suitable aging methods for building their own mock-up systems, and to encourage the development of more sustainable aging protocols for future conservation of historical silver objects.</p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"5 5","pages":""},"PeriodicalIF":6.1,"publicationDate":"2025-02-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202400055","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143945035","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Sandesh Chickmagalur Jatheendranath, Akhi Das, Sudhindra H Deshpande, Nilamoni Nath, Walter Maier, Verena Streitferdt, Udaya Kiran Marelli
{"title":"Graphene Oxide-Cyclopentylamine (GO-d-CP) Liquid Crystals as a Novel Alignment Medium for Anisotropic NMR with Analyte Recovery","authors":"Sandesh Chickmagalur Jatheendranath, Akhi Das, Sudhindra H Deshpande, Nilamoni Nath, Walter Maier, Verena Streitferdt, Udaya Kiran Marelli","doi":"10.1002/cmtd.202400039","DOIUrl":"https://doi.org/10.1002/cmtd.202400039","url":null,"abstract":"<p>In this study, we present graphene oxide derivatized with cyclopentylamine (GO-d-CP) as a DMSO-compatible liquid crystal alignment medium that is free from any background NMR signal for application in anisotropic NMR. This novel alignment medium facilitates optimal isotropic and anisotropic conditions within a single sample preparation, controlled by sonication, thereby enabling the measurement of anisotropic NMR parameters- residual dipolar couplings (RDC) and residual chemical shift anisotropy (RCSA). GO-d-CP offers several advantages, including ease of synthesis, isolation of solid GO-d-CP as a stable non-hygroscopic material, and maintenance of the anisotropic state stability >30 days, allowing for prolonged and repetitive experiments. Notably, post the analysis it allows for easy recovery of valuable analytes as well as GO-d-CP for reuse, enabling the routine application of anisotropic NMR in structural analysis of small molecules. We demonstrate its efficacy by analyzing the relative stereochemistry of four compounds - estrone, santonin, griseofulvin, and cinmethylin - using anisotropic NMR data.</p>","PeriodicalId":72562,"journal":{"name":"Chemistry methods : new approaches to solving problems in chemistry","volume":"5 4","pages":""},"PeriodicalIF":6.1,"publicationDate":"2025-02-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cmtd.202400039","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143793481","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}