TY - JOUR
A1 - Stolar, Tomislav
A1 - Alić, Jasna
A1 - Casali, Lucia
A1 - Gugin, Nikita
A1 - Baláž, Matej
A1 - Michalchuk, Adam
A1 - Emmerling, Franziska
ED - Stolar, Tomislav
T1 - Mechanochemistry: Looking back and ahead
N2 - Starting with the discovery of fire and the preparation of food in prehistoric times, mechanochemistry is the oldest form of chemistry that humans have controlled. Mechanochemical practices, such as grinding with a mortar and pestle, continued into the Middle Ages until dedicated scientific studies began in the 19th century. Since then,research in mechanochemistry has shown that many chemicalreactions can be performed via mechanical force without or with small amounts of solvent. Besides being time, material, and energy efficient, mechanochemical reactions often yield products that differ from those obtained in solution. Therefore, not only is mechanochemistry greener and more sustainable than conventional solution chemistry, but it also has the added value of providing new reactivity and selectivity. This is especially important today, when chemists need to invent high-performance materials, intermediates, and products with the use of sustainable feedstocks and develop environmental remediation pathways. At the same time, time-resolved in situ monitoring and computational modeling are necessary for addressing fundamental questions about the atomistic, molecular, and electronic nature of mechanochemical reactivity. Integrating digitalization, robotics, and artificial intelligence tools promises to increase the reproducibility and scalability of mechanochemical processes. Further evolution of mechanochemistry is expected to have a transformative effect on the chemical industry.
KW - Mechanochemistry
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653962
DO - https://doi.org/10.1016/j.chempr.2025.102880
SN - 2451-9294
VL - 12
IS - 2
SP - 1
EP - 27
PB - Elsevier BV
AN - OPUS4-65396
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Stolar, Tomislav
A1 - Bayram, Dilara
A1 - May, Anastasia
A1 - Sundermann, Remie
A1 - Prinz, Carsten
A1 - Meyer, Klas
A1 - Myxa, Anett
A1 - Falkenhagen, Jana
A1 - Emmerling, Franziska
T1 - Selective mechanochemical conversion of post-consumer polyethylene terephthalate waste into hcp and fcu UiO-66 metal–organic frameworks
N2 - Single-use plastics strongly contribute to plastic pollution, and less than 10% of plastic waste is recycled globally. Here, we present a selective mechanochemical protocol for converting post-consumer polyethylene terephthalate (PET) transparent bottles and coloured textile waste into the porous metal–organic framework (MOF) UiO-66 materials. We used time-resolved in situ (TRIS) synchrotron powder X-ray diffraction and Raman spectroscopy to monitor the depolymerization of PET during ball milling. To convert disodium terephthalate to UiO-66, we developed base and base-free synthetic routes that lead to fcu and hcp UiO-66 phases, respectively, including the first ever synthesis of hcp UiO-66 by mechanochemistry. Our results demonstrate the potential of mechanochemistry to selectively access fcu and hcp UiO-66 phases using post-consumer PET waste.
KW - Mechanochemistry
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653958
DO - https://doi.org/10.1039/D4MR00126E
SN - 2976-8683
SP - 1
EP - 8
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-65395
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Gugin, Nikita
A1 - Schwab, Alexander
A1 - Carraro, Francesco
A1 - Tavernaro, Isabella
A1 - Falkenhagen, Jana
A1 - Villajos, Jose
A1 - Falcaro, Paolo
A1 - Emmerling, Franziska
T1 - ZIF-8-based biocomposites via reactive extrusion: towards industrial-scale manufacturing
N2 - Mechanochemistry, a sustainable synthetic method that minimizes solvent use, has shown great promise in producing metal–organic framework (MOF)-based biocomposites through ball milling. While ball milling offers fast reaction times, biocompatible conditions, and access to previously unattainable biocomposites, it is a batch-type process typically limited to gram-scale production, which is insufficient to meet commercial capacity. We introduce a scalable approach for the continuous solid-state production of MOF-based biocomposites. Our study commences with model batch reactions to examine the encapsulation of various biomolecules into Zeolitic Imidazolate Framework-8 (ZIF-8) via hand mixing, establishing a foundation for upscaling. Subsequently, the process is scaled up using reactive extrusion, enabling continuous and reproducible kilogram-scale production of bovine serum albumin (BSA)@ZIF-8 with tunable protein loading. Furthermore, we achieve the one-step formation of shaped ZIF-8 extrudates encapsulating clinical therapeutic hyaluronic acid (HA). Upon release of HA from the composite, the molecular weight of HA is preserved, highlighting the industrial potential of reactive extrusion for the cost-effective and reliable manufacturing of biocomposites for drug-delivery applications.
KW - Mechanochemistry
KW - Extrusion
KW - Biocompoites
KW - MOFs
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-654777
DO - https://doi.org/10.1039/D5TA08276E
SN - 2050-7496
SP - 1
EP - 14
PB - Royal Society of Chemistry
AN - OPUS4-65477
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Krause, Christina
A1 - Szymoniak, Paulina
A1 - Lohstroh, W.
A1 - Juranyi, F.
A1 - Zamponi, M.
A1 - Frick, B.
A1 - Al-Sabbagh, Dominik
A1 - Emmerling, Franziska
A1 - Zorn, R.
A1 - Schönhals, Andreas
T1 - Complex molecular dynamics of symmetric model discotic liquid crystals: Comparison of Hexakis(hepta-alkanoyloxy)triphenylene (HOT6) with Hexakis(hexa-alkyloxy)triphenylene (HAT6)
N2 - This study investigates the complex molecular dynamics of discotic liquid crystals (DLCs) by comparing two structurally similar compounds: Hexakis(hepta-alkanoyloxy)triphenylene (HOT6) and Hexakis(hexa-alkyloxy)triphenylene (HAT6) having the same triphenyl core and the same length of the alkyl side chain. The difference of both materials is that the alkyl chain is linked by an oxygen bridge to the triphenylene core for HAT6 and by a ester group for HOT6. Using a combination of broadband dielectric spectroscopy, differential scanning calorimetry, X-ray scattering, and neutron scattering techniques, the research explores the glass transition phenomena and relaxation processes in these materials. HOT6, featuring ester linkages, exhibits distinct dynamic behavior compared to HAT6, including two separate glass transitions indicated by the 1- and 2-relaxation found by dielectric spectroscopy which are assigned to the glassy dynamics of the alkyl side chain in the intercolumnar space and that of the columns, respectively. The study reveals that the ester group in HOT6 leads to increased molecular rigidity and altered packing in the intercolumnar space, as evidenced by X-ray scattering and the vibrational density of states. Neutron scattering confirms localized methyl group rotations and a further relaxation process which relates to the -relaxation revealed by dielectric spectroscopy. The findings contribute to a deeper understanding of glassy dynamics in partially ordered systems and highlight the influence of molecular architecture on relaxation behavior in DLCs.
KW - Discotic Liquid Crystals
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655171
DO - https://doi.org/10.1039/d5sm01247c
SN - 1744-6848
SP - 1
EP - 17
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-65517
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Pavlidis, Sotirios
A1 - Fischer, Eric W.
A1 - Opis-Basilio, Amanda
A1 - Bera, Ayan
A1 - Guilherme Buzanich, Ana
A1 - Álvarez-Sánchez, María
A1 - Wittek, Severin
A1 - Emmerling, Franziska
A1 - Ray, Kallol
A1 - Roemelt, Michael
A1 - Abbenseth, Josh
T1 - Ambiphilic Reactivity and Switchable Methyl Transfer at a T-Shaped Bi(NNN) Complex Enabled by a Redox-Active Pincer Ligand
N2 - We report the transition-metal-like reactivity of a geometrically constrained, ambiphilic bismuth(III) trisamide. Planarization of the Bi(III) center unlocks Bi−C bond formation when reacted with mild electrophiles (alkyl iodides and triflates) accompanied by two-electron oxidation of the utilized NNN pincer nligand. The preservation of the bismuth oxidation state is confirmed by single-crystal X-ray diffraction and X-ray absorption spectroscopy and corroborated by theoretical calculations. Sequential reduction of the oxidized ligand framework alters the reactivity of a generated Bi−Me unit, enabling controlled access to methyl cation, radical, and anion equivalents. The full [Bi(Me)(NNN)]+/•/− redox series was comprehensively characterized using NMR and EPR spectroscopy as well as spectro-electrochemistry. This work represents the first example of ligand-assisted, redox-neutral C−X bond splitting at bismuth, establishing a new paradigm for synthetic bismuth chemistry.
KW - Pincer ligand
KW - XAS
KW - Redox
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-654948
DO - https://doi.org/10.1021/jacs.5c18955
SN - 0002-7863
VL - 148
IS - 2
SP - 2683
EP - 2692
PB - American Chemical Society (ACS)
AN - OPUS4-65494
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Chakraborty, Gouri
A1 - Das, Prasenjit
A1 - Bhattacharya, Biswajit
A1 - Prinz, Carsten
A1 - Emmerling, Franziska
A1 - Thomas, Arne
T1 - Room-temperature superprotonic conductivity in COOH-functionalized multicomponent covalent organic frameworks
N2 - In solid materials, the development of hydrogen bonding (H-bonding) networks within pores is crucial for efficient proton conductance. In this study, a chemically stable carboxylic acid-functionalized, quinoline-linked 2D microporous covalent organic framework (COF) (Qy-COOH) was synthesized using the Doebner multicomponent reaction (MCR) and compared to a similar framework lacking the –COOH functionality (Qy-H), prepared via an MC Domino reaction. The proton conductivity of the –COOH-functionalized MCR-COF was significantly enhanced, reaching 10−2 S cm−1, attributed to strong H-bonding interactions between water molecules and the dangling –COOH groups within the COF pores. In contrast, the analogous Qy-H framework exhibited a much lower proton conductivity of 10−5 S cm−1, while an imine-based COF showed only 10−6 S cm−1. This work represents the first demonstration of a general strategy to achieve efficient proton conduction in a class of layered 2D –COOH-functionalized COFs, offering superprotonic conductivity without requiring additives at room temperature. The MCR-COF design approach provides a promising pathway for developing highly stable and high-performance proton-conducting materials.
KW - Multicomponebt
KW - COF
KW - Proton Conductivity
KW - Superprotonic
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653526
DO - https://doi.org/10.1039/D5SC06953J
SN - 2041-6520
SP - 1
EP - 9
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-65352
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Hickel, Tilmann
A1 - Waske, Anja
A1 - Tehranchi, Ali
A1 - Bhattacharya, Biswajit
A1 - Stawski, Tomasz M.
A1 - Fellinger, Tim-Patrick
A1 - Mehmood, Asad
A1 - Witt, Julia
A1 - Ozcan, Ozlem
A1 - Guilherme Buzanich, Ana
A1 - Kumar, Sourabh
A1 - Mishra, Rajesh Kumar
A1 - Holzer, Marco
A1 - Stucchi de Camargo, Andrea Simone
A1 - Agudo Jácome, Leonardo
A1 - Manzoni, Anna
A1 - Fantin, Andrea
A1 - John, Elisabeth
A1 - Hodoroaba, Vasile-Dan
A1 - Bührig, Sophia
A1 - Murugan, Jegatheesan
A1 - Marschall, Niklas
A1 - George, Janine
A1 - Darvishi Kamachali, Reza
A1 - Maaß, Robert
A1 - Emmerling, Franziska
T1 - Chemically complex materials enable sustainable high-performance materials
N2 - Chemically complex materials (CCMats) including high-entropy alloys, oxides, and related multi-principal element systems offer a paradigm shift in materials design by leveraging chemical diversity to simultaneously optimize functional, structural, and sustainability criteria. The vastness of the compositional and structural space in CCMats propels the field into an expanding exploratory state. To reconcile functional and structural performance across this immense parameter space remains an open challenge. This Perspective evaluates the opportunities and challenges associated with harnessing chemical complexity across a broad spectrum of applications, such as hydrogen storage, ionic conductors, catalysis, magnetics, dielectrics, semiconductors, optical materials, and multifunctional structural systems. It is delineated how three central design strategies: targeted substitution (SUB), defect engineering (DEF), and diversity management (DIV) enable the reconciliation of high functional performance with long-term structural stability and environmental responsibility.
Advances in computational thermodynamics, microstructure simulations, machine learning, and multimodal characterization are accelerating the exploration and optimization of CCMats, while robust data infrastructures and automated synthesis workflows are emerging as essential tools for navigating their complex compositional space. By fostering cross-disciplinary knowledge transfer and embracing data-driven design, CCMats are poised to deliver next-generation materials solutions that address urgent technological, energy, and
environmental demands.
KW - Chemically complex materials
KW - Structural stability
KW - Functional performance
KW - Design strategies
KW - Sustainability
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655598
UR - https://www.sciencedirect.com/science/article/pii/S1359028626000033?via%3Dihub
DO - https://doi.org/10.1016/j.cossms.2026.101256
SN - 1359-0286
VL - 42
SP - 1
EP - 26
PB - Elsevier Ltd.
CY - Amsterdam
AN - OPUS4-65559
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Rodríguez‐Sánchez, Noelia
A1 - Ballesteros, Menta
A1 - Prinz, Carsten
A1 - Canosa, Inés
A1 - Flores Díaz, Amando
A1 - Bhattacharya, Biswajit
A1 - Ruiz‐Salvador, A. Rabdel
A1 - Emmerling, Franziska
T1 - Mechanochemical Fullerene Nanoencapsulation in Amino‐Functionalized ZIF‐12 for Visible‐Light Disinfection of Waterborne Viruses and Bacteria
N2 - Water contamination poses a significant threat to public health and environmental sustainability, necessitating the development of efficient purification technologies. This study reports the mechanochemical synthesis of an amino-functionalized ZIF 12 framework with encapsulated fullerene (C60) as a bifunctional photocatalyst for water decontamination and disinfection under visible-light irradiation. The samples were characterized using powder X-ray diffraction (PXRD), FT-IR spectroscopy, N2 adsorption isotherm, X-ray photoelectron spectroscopy (XPS), electron microscopy (SEM and TEM), thermogravimetric Analysis (TGA), and UV–vis diffuse reflectance spectroscopy (DRS), confirming the retention of crystallinity and effective incorporation of C60 and amino groups within the framework. Fullerene loading and amino functionalization modified the optical properties, extending visible light absorption and enhancing charge separation and photocatalytic activity. The synergistic interaction between amino groups and C60 promotes efficient charge separation and enhanced hydroxyl radical production, resulting in improved photocatalytic and photo-Fenton activity. C60@ZIF-12-NH2 exhibited excellent photocatalytic performance, achieving the completeinactivation of bacteriophage P22 under saline conditions and effective disinfection of E.coli and coliforms innatural river water, demonstrating robustness under environmentally relevant conditions. The solvent-minimized mechanochemical synthesis and visible-light-driven activity position the C60@ZIF-12-NH2 composite as a promising platform for sustainable and advanced water treatment applications.
KW - Fullerene
KW - Heterogeneous photo-Fenton
KW - Mechanochemistry
KW - Nanoencapsulation
KW - Photocatalysis
KW - ZIF-12
PY - 2026
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-656531
DO - https://doi.org/10.1002/smll.202512881
SN - 1613-6810
SP - 1
EP - 19
PB - Wiley-VCH GmbH
AN - OPUS4-65653
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Dolai, Malay
A1 - Saha, Urmila
A1 - Goswami, Juli Nanda
A1 - Bhattacharya, Biswajit
A1 - Emmerling, Franziska
A1 - Ifseisi, Ahmad A.
A1 - Biswas, Surajit
ED - Bhattacharya, Biswajit
T1 - Nickel(II)-mediated in situ complex formation with unexpected ligand transformations: crystal structures, DFT calculations, and catalytic activity in CO2 fixation reactions
N2 - Two transformed ligands, namely 1,3,5-triazapentadienato(imidoylamidinato) and N-(methoxy(pyrimidin-2-yl)(pyrimidine-2-carboxamido)methyl)pyrimidine-2-carboxamide, are reported here as the first products derived from 2-cyano pyridine/pyrimidine, respectively, under nickel metal mediation in the presence of hydroxylamine hydrochloride in situ. Two different nickel-coordinated complexes (1 and 2) were formed. Single crystal X-ray diffraction revealed that complex 1 is a mononuclear complex with tetra-coordinated square planar geometry, whereas complex 2 is a dinuclear complex with hexa-coordinated distorted octahedral geometry. The synthetic pathways of both transformed ligands are explained with the support of energy calculations of different states via density functional theory (DFT) calculations. The catalytic addition reactions of epoxides and carbon dioxide efficiently produce organic cyclic carbonates in the presence of complexes 1–2, attributed to the presence of Lewis acidic nickel and Lewis basic centers, such as free amine, imine, methoxy, or nitrogen in complexes 1 and 2. Under mild reaction conditions (1 atm CO2 pressure and 60 °C temperature), different types of epoxides (exocyclic, endocyclic, and aromatic epoxides) yield high levels of respective cyclic carbonates in the presence of both complexes 1–2 as catalysts, with tert-butylammonium bromide (TBAB) acting as a co-catalyst. The high turnover number (TON) and turnover frequency (TOF) of these catalytic reactions clearly indicate the efficacy of the two catalysts.
KW - Catalytic activity in CO2 fixation reactions DFT calculations
KW - Nickel(II)-complex
KW - In situ complex formation
KW - Crystal Structure
PY - 2025
DO - https://doi.org/10.1039/d4nj01801j
SN - 1369-9261
VL - 49
IS - 11
SP - 4451
EP - 4463
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-62782
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Heinekamp, Christian
A1 - Palmer, Tahlia M.
A1 - Al‐Sabbagh, Dominik
A1 - May, Anastasia
A1 - Prinz, Carsten
A1 - Michalik, Stefan
A1 - Michalchuk, Adam
A1 - Emmerling, Franziska
T1 - Pre‐Activation as a Route for Tuning the Kinetics of Mechanochemical Transformations
N2 - Learning to control reaction kinetics is essential for translating any chemical technology into real‐world application. Based on time‐resolved in situ powder X‐ray diffraction data, we demonstrate the opportunity to tune mechanochemical reaction rates through the pre‐activation of the starting reagents. For three model co‐crystal systems, the pre‐activation of the most stable reagent yields up to a ca 10‐fold increase in the reaction rate, whilst negligible kinetic enhancement is seen when the less stable reagent is pre‐activated. Moreover, we demonstrate how the polymorphic outcome of mechano‐co‐crystallization is also sensitive to pre‐activation of the starting material. Our results suggest that reproducibility of mechanochemical processes requires detailed understanding over the origin and history of reagent powders, whilst providing a new conceptual framework to design and control mechanochemical reactions.
KW - Mechanochemistry
KW - In situ synthesis
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-649409
DO - https://doi.org/10.1002/anie.202516632
SN - 1433-7851
SP - 1
EP - 7
PB - Wiley VHC-Verlag
AN - OPUS4-64940
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Speight, Isaiah R.
A1 - Ardila-Fierro, Karen J.
A1 - Hernández, José G.
A1 - Emmerling, Franziska
A1 - Michalchuk, Adam
A1 - García, Felipe
A1 - Colacino, Evelina
A1 - Mack, James
T1 - Ball milling for mechanochemical reactions
N2 - Mechanochemistry is an emerging field with the potential to pave the way for sustainable chemistry. Although the use of mechanical force to initiate chemical reactions has been recognized for millennia, it has often taken a backseat to thermal and photonic methods. Over the past 30 years, mechanochemistry has seen a resurgence of interest, attracting researchers across the globe. Despite its proven ability to address numerous challenges within the chemical community, mechanochemistry remains on the periphery. This Primer serves as a valuable guide for conducting mechanochemical reactions by ball milling, offering an overview of the processes, methods, tools and terminology necessary to embark on research in this field. It also highlights persistent hurdles such as equipment standardization, understanding the impact of new discoveries and the lack of predictability of reaction outcomes. The Primer’s focus is on how mechanochemical ball milling is used in various chemical transformations, distinguishing it from other forms of mechanochemistry discussed in the literature. With a promising future, this Primer serves as a gateway for those aspiring to contribute to the field’s advancement.
KW - Mechanochemistry
KW - Ball milling
KW - Upscaling
PY - 2025
DO - https://doi.org/10.1038/s43586-025-00401-2
SN - 2662-8449
VL - 5
IS - 1
SP - 1
EP - 18
PB - Springer Science and Business Media LLC
AN - OPUS4-63447
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Starkholm, A.
A1 - Al-Sabbagh, Dominik
A1 - Sarisozen, S
A1 - von Reppert, A
A1 - Rössle, M
A1 - Ostermann, Markus
A1 - Unger, E
A1 - Emmerling, Franziska
A1 - Kloo, L
A1 - Svensson, P
A1 - Lang, F
A1 - Maslyanchuk, O.
T1 - Green Fabrication of Sulfonium-Containing Bismuth Materials for High-Sensitivity X-Ray Detection
N2 - Organic–inorganic hybrid materials based on lead and bismuth have recently been proposed as novel X- and gamma-ray detectors for medical imaging, non-destructive testing, and security, due to their high atomic numbers and facile preparation compared to traditional materials like amorphous selenium and Cd(Zn)Te. However, challenges related to device operation, excessively high dark currents, and long-term stability have delayed commercialization. Here, two novel semiconductors incorporating stable sulfonium cations are presented, [(CH3CH2)3S]6Bi8I30 and [(CH3CH2)3S]AgBiI5, synthesized via solvent-free ball milling and fabricated into dense polycrystalline pellets using cold isostatic compression, two techniques that can easily be upscaled, for X-ray detection application. The fabricated detectors exhibit exceptional sensitivities (14 100–15 190 µC Gyair−1 cm−2) and low detection limits (90 nGyair s−1 for [(CH3CH2)3S]6Bi8I30 and 78 nGyair s−1 for [(CH3CH2)3S]AgBiI5), far surpassing current commercial detectors. Notably, they maintain performance after 9 months of ambient storage. The findings highlight [(CH3CH2)3S]6Bi8I30 and [(CH3CH2)3S]AgBiI5 as scalable, cost-effective and highly stable alternatives to traditional semiconductor materials, offering great potential as X-ray detectors in medical and security applications.
KW - Mechanochemistry
KW - X-ray detectors
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630306
DO - https://doi.org/10.1002/adma.202418626
SP - 1
EP - 10
PB - Wiley VHC-Verlag
AN - OPUS4-63030
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Rodríguez-Sánchez, Noelia
A1 - Bhattacharya, Biswajit
A1 - Emmerling, Franziska
A1 - Prinz, Carsten
A1 - Prieto-Laria, P.
A1 - Ruiz-Salvador, A.R.
A1 - Ballesteros, M.
T1 - Engineering a multivariate cobalt metal–organic framework for high photocatalytic activity: the impact of mixed ligands and metal incorporation in a visible light-driven heterogeneous photo-Fenton reaction for water treatment
N2 - Metal–organic frameworks (MOFs) have attracted increasing attention for the removal of organic pollutants in wastewater via photocatalysis. Here, we design a multivariate modification of ZIF-9 to tune its electronic properties for use in visible light photocatalysis. A controllable synthesis of ZIF-9 and its multivariate forms with the incorporation of copper and the 2-imidazolecarboxaldehyde (ica) ligand was carried out. The materials are tested for the removal of the model dye methylene blue (MB) by a heterogeneous photo-Fenton-like reaction at neutral pH and room temperature. Cu-ZIF-9-ica (UPO-3) shows high photocatalytic activity under both visible and ultraviolet A (UVA) light, achieving 94% MB degradation in 45 min, compared to 65% MB degradation in 120 min using bare ZIF-9. The study revealed a first-order rate constant of 0.0475 min−1 for Cu-ZIF-9-ica compared to 0.0088 min−1 for ZIF-9 under visible light. The improvement of the catalyst was clearly attributed to the co-incorporation of Cu and the ica ligand in the MOF, which reduces the band gap, in agreement with DFT calculations. Reproducibility and recyclability tests proved that Cu-ZIF-9-ica can be used for at least 3 cycles without a significant loss of efficiency, making it a promising material for the study and application of wastewater treatment.
KW - Metal-Organic Framework (MOF)
KW - Heterogeneous photo-Fenton
KW - ZIF-9
KW - Methylene Blue
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630797
DO - https://doi.org/10.1039/d4na00954a
SN - 2516-0230
VL - 7
IS - 8
SP - 2255
EP - 2265
PB - Royal Society of Chemistry
AN - OPUS4-63079
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Liu, Yanchen
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Montoro, Luciano A.
A1 - Liu, Hao
A1 - Liu, Ye
A1 - Emmerling, Franziska
A1 - Russo, Patrícia A.
A1 - Pinna, Nicola
T1 - A partially disordered crystallographic shear block structure as fast-charging negative electrode material for lithium-ion batteries
N2 - A well-ordered crystalline structure is crucial in battery electrodes, as the dimensionality and connectivity of the interstitial sites inherently influence Li+ ions diffusion kinetics. Niobium tungsten oxides block structures, composed of ReO3-type blocks of specific sizes with well-defined metal sites, are promising fast-charging negative electrode materials. Structural disorder is generally detrimental to conductivity or ion transport. However, here, we report an anomalous partially disordered Nb12WO33 structure that significantly enhances Li-ion storage performance compared to the known monoclinic Nb12WO33 phase. The partially disordered phase consists of corner-shared NbO6 octahedra blocks of varied sizes, including 5×4, 4×4, and 4×3, with a disordered arrangement of distorted WO4 tetrahedra at the corners of the blocks. This structural arrangement is robust during lithiation/delithiation, exhibiting minor local structure changes during cycling. It enables accelerated Li-ion migration, resulting in promising fast-charging performance, namely, 62.5 % and 44.7 % capacity retention at 20 C and 80 C, respectively. This study highlights the benefits of introducing disorder into niobium tungsten oxide shear structures, through the establishment of clear structure-performance correlations, offering guidelines for designing materials with targeted properties.
KW - Lithium ion batteries
KW - Oxides
KW - XANES
KW - XRD
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637994
DO - https://doi.org/10.1038/s41467-025-61646-9
SN - 2041-1723
VL - 16
IS - 1
SP - 1
EP - 15
PB - Springer Science and Business Media LLC
AN - OPUS4-63799
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Heinekamp, Christian
A1 - Roy, Arkendu
A1 - Karafiludis, Stephanos
A1 - Kumar, Sourabh
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Stawski, Tomasz M.
A1 - Miliūtė, Aistė
A1 - von der Au, Marcus
A1 - Ahrens, Mike
A1 - Braun, Thomas
A1 - Emmerling, Franziska
T1 - Zirconium fluoride-supported high-entropy fluoride: a catalyst for enhanced oxygen evolution reaction
N2 - Extended hydrogen initiatives promote the urgency of research on water splitting technologies and, therein, oxygen evolution reaction catalysts being developed. A route to access a ZrF4 supported high-entropy fluoride catalyst using a facile sol–gel route is presented. The high-entropy character of the catalyst was confirmed by scanning transmission electron microscopy and energy dispersive X-ray spectroscopy (STEM-EDX) as well as inductively coupled plasma-mass spectrometry (ICP-MS). Additional investigations on the local structure were performed using extended X-ray absorption fine structure spectroscopy (EXAFS) and pair distribution function (PDF) analysis. The catalyst shows significant potential for oxygen evolution reaction (OER) in alkaline media with a current density of 100 mA cm−2 at approximately 1.60 V, thus outperforming benchmark materials such as IrO2, despite a significant reduction in electrochemical mass loading. A potential mechanism is suggested based on free energy calculation using DFT calculations.
KW - OER
KW - HEA
KW - CCMAT
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637116
DO - https://doi.org/10.1039/D4TA08664C
SN - 2050-7488
VL - 13
IS - 26
SP - 20383
EP - 20393
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-63711
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Das, Prasenjit
A1 - Chakraborty, Gouri
A1 - Yang, Jin
A1 - Roeser, Jérôme
A1 - Küçükkeçeci, Hüseyin
A1 - Nguyen, Anh Dung
A1 - Schwarze, Michael
A1 - Gabriel, Jose
A1 - Penschke, Christopher
A1 - Du, Shengjun
A1 - Weigelt, Vincent
A1 - Khalil, Islam E.
A1 - Schmidt, Johannes
A1 - Saalfrank, Peter
A1 - Oschatz, Martin
A1 - Rabeah, Jabor
A1 - Schomäcker, Reinhard
A1 - Emmerling, Franziska
A1 - Thomas, Arne
T1 - The Effect of Pore Functionality in Multicomponent Covalent Organic Frameworks on Stable Long‐Term Photocatalytic H2 Production
N2 - AbstractIn nature, organic molecules play a vital role in light harvesting and photosynthesis. However, regarding artificial water splitting, the research focus is primarily on inorganic semiconductors. Although organic photocatalysts have high structural variability, they tend to exhibit lower quantum efficiencies for water splitting than their inorganic counterparts. Multicomponent reactions (MCRs) offer an attractive route to introduce different functional units into covalent organic frameworks (COFs) and enable semiconducting properties and high chemical stability, creating promising materials for long‐term photocatalytic applications, such as H2 production. Herein, five highly crystalline donor‐acceptor based, 4‐substituted quinoline‐linked MCR‐COFs are presented that are prepared via the three‐component Povarov reaction. The pore functionality is varied by applying different vinyl derivatives (e.g., styrene, 2‐vinyl pyridine, 4‐vinylpyridine, 4‐vinyl imidazole, 2,3,4,5,6‐pentafluorostyrene), which has a strong influence on the obtained photocatalytic activity. Especially an imidazole‐functionalized COF displays promising photocatalytic performance due to its high surface area, crystallinity, and wettability. These properties enable it to maintain its photocatalytic activity even in a membrane support. Furthermore, such MCR‐COFs display dramatically enhanced (photo)chemical stability even after long‐term solar light irradiation and exhibit a high and steady H2 evolution for at least 15 days.
KW - Sstability
KW - Covalent organic frameworks
KW - Pore functionality
KW - Long-term H2 production
KW - Multicomponent reactions
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639787
DO - https://doi.org/10.1002/aenm.202501193
SN - 1614-6832
SP - 1
EP - 10
PB - Wiley VHC-Verlag
AN - OPUS4-63978
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Rodríguez-Sánchez, Noelia
A1 - Domínguez-Santos, J. Enrique
A1 - Bhattacharya, Biswajit
A1 - Prinz, Carsten
A1 - Canosa, Inés
A1 - Flores, Amando
A1 - Jiménez-Rodríguez, Antonia
A1 - Ruiz-Salvador, A. Rabdel
A1 - Emmerling, Franziska
A1 - Ballesteros, Menta
T1 - Mechanochemical synthesis of multivariate UPO-3 (Cu-ZIF-9-ica) MOF for inactivation of antibiotic-resistant bacteria and irrigation-quality water production via heterogeneous photo-Fenton catalysis
N2 - Water scarcity and pollution are critical global challenges, particularly in agriculture, the largest consumer of water. The development of sustainable, effective, and environmentally friendly disinfection methods is essential to address the risks posed by antibiotic-resistant bacteria and to ensure safe reuse of water for irrigation. In this study, we report the synthesis of the metal-organic framework (MOF) Universidad Pablo de Olavide-3 (UPO-3) via a mechanochemical approach, a scalable and sustainable method compared to traditional solvothermal synthesis. The resulting UPO-3/H2O2 system exhibits robust photocatalytic properties under visible light, achieving effective and broad-spectrum antibacterial activity. The disinfection efficiency of the catalyst was evaluated against Escherichia coli as a model of microbial pathogen in two saline matrices, considering the key parameters of the heterogeneous photo-Fenton process, including catalyst dosage, initial H2O2 concentration, and light irradiation. Notably, it inactivated two important virulent and antibiotic-resistant bacterial pathogens (Staphylococcus aureus and Pseudomonas aeruginosa). Furthermore, UPO-3 shows exceptional performance under real-world conditions, such as river water disinfection, achieving >5-log reduction of E. coli, fulfilling a critical criterion for Class A water reuse under Regulation (EU) 2020/741. These results highlight UPO-3 as a versatile and sustainable solution for water reuse, addressing water scarcity and advancing efforts to achieve United Nations Sustainable Development Goal 6.
KW - Water reuse
KW - Antibiotic-resistant bacteria
KW - Water disinfection
KW - Mechanochemical synthesis
KW - Metal organic framework
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639766
DO - https://doi.org/10.1016/j.chemosphere.2025.144610
SN - 0045-6535
VL - 386
SP - 1
EP - 11
PB - Elsevier Ltd.
AN - OPUS4-63976
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Go, Eun Sul
A1 - Hong, Eun Ji
A1 - Lee, Ji Yeong
A1 - Stolar, Tomislav
A1 - Peterson, Gregory I.
A1 - Emmerling, Franziska
A1 - Kim, Kyoungsoo
A1 - Kim, Jeung Gon
T1 - Insights into Mechanochemical Solid-State Ball-Milling Reaction: Monitoring Transition from Heterogeneous to Homogeneous Conditions
N2 - As mechanochemical synthesis has advanced significantly, there has been intense interest in understanding the underlying mechanisms of these reactions. Given that many mechanochemical processes are conducted in the solid-state without solvation yet sometimes yield faster reactions than those in solution, we sought to address the following question: Are mechanochemical reactions homo- or heterogeneous? To investigate, we employed a model system involving the mixing and copolymerization of l-lactide (LLA) and d-lactide (DLA), monitored through powder X-ray diffraction (PXRD), nuclear magnetic resonance, and differential scanning calorimetry. In situ and ex situ PXRD analyses of the mixture of LLA and DLA showed that vibratory ball milling rapidly transformed the initially heterogeneous lactide mixture into a homogeneous phase within one min due to collisions between the balls and the jar. By varying the milling conditions, we were able to regulate the level of mixing, which subsequently influenced the copolymerization outcomes. In the solid-state ball-milling copolymerization of LLA and DLA in the presence of a catalyst and initiator, multiblock copolymers of poly(l-lactic acid) and poly(d-lactic acid) were formed within one min during the early stage of the reaction, when incomplete mixing of the monomers led to a process governed by phase heterogeneity. In contrast, prolonged polymerization promoted conditions approaching homogeneity, ultimately yielding atactic poly(lactic acid). This transition from heterogeneous to homogeneous reactions is a distinctive feature compared to conventional homogeneous reactions, potentially leading to mechano-exclusive reaction designs.
KW - Mechanochemistry
KW - Ball-milling
KW - Homogeneous reaction
KW - Heterogeneous reaction
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638008
DO - https://doi.org/10.1021/jacsau.5c00322
SN - 2691-3704
VL - 5
IS - 6
SP - 2720
EP - 2727
PB - American Chemical Society (ACS)
AN - OPUS4-63800
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Fink, Friedrich
A1 - Stawski, Tomasz M.
A1 - Emmerling, Franziska
A1 - Falkenhagen, Jana
T1 - A novel machine-learning approach to unlock technical lignin classification by NIR spectroscopy - bench to handheld
N2 - In this research, the utilization of near-infrared (NIR) spectroscopy in conjunction with advanced machine learning methods is investigated for categorizing technical lignins obtained from different biomass sources and industrial procedures. Technical lignins, such as kraft, organosolv and lignosulfonates, have different chemical compositions, which continue to make uniform characterization and application in sustainable sectors extremely difficult. Fast, universally accessible analytics combined with data analysis is still an open question. For the first time three distinct NIR spectrometers—a high-performance benchtop system, a mid-priced compact device, and an economical handheld unit—were utilized to record NIR spectra of 31 unique lignin samples. The spectra underwent pre-processing through standard normal variate (SNV) transformation and Savitzky-Golay derivatives to amplify spectral features and decrease noise. Principal component analysis (PCA) was employed to reduce data complexity and extract crucial characteristics for classification purposes. Subsequently, four machine learning algorithms—Support Vector Machines (SVM), Gaussian Naive Bayes (GNB), Gaussian Process Classification (GPC), and Decision Tree Classification (DTC)—were implemented for the classification of the lignin samples. The DTC model exhibited the highest accuracy among them across different spectrometers. Although the benchtop spectrometer produced the most precise outcomes, the compact NeoSpectra system also displayed potential as a cost-efficient option. Nonetheless, the restricted spectral coverage of the handheld NIRONE spectrometer resulted in reduced classification accuracy. Our discoveries highlight the capability of NIR spectroscopy, combined with robust data analysis techniques, for the swift and non-destructive classification of technical lignins, facilitating their improved utilization in sustainable fields.
KW - Technical lignins
KW - NIR spectroscopy
KW - Classification
KW - Machine-learning
KW - PCA
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634518
DO - https://doi.org/10.1016/j.chemolab.2025.105467
SN - 0169-7439
VL - 264
SP - 1
EP - 10
PB - Elsevier B.V.
CY - Amsterdam
AN - OPUS4-63451
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Feiler, Torvid
A1 - Emmerling, Franziska
A1 - Bhattacharya, Biswajit
T1 - Sustainable mechanochemical approach for the selective synthesis of multicomponent organic solids: real-time in situ insights
N2 - Crystalline multicomponent organic solids (MOSs) such as cocrystals and ionic cocrystals hold immense potential in diverse functional applications, ranging from pharmaceuticals to optoelectronics. However, conventional solution-based crystallization methods often result in polymorphic mixtures and lack precise control over product composition. Herein, we report a comparative investigation of solution crystallization versus mechanochemical synthesis for constructing MOSs from 9-anthracenecarboxylic acid (ACA) and 4,4 '-bipyridine (BPY). Solution-based approaches consistently yielded concomitant formation of neutral cocrystal (CC) and ionic cocrystal (ICC) forms, regardless of the solvent used. The resulting multicomponent solids were comprehensively characterized using a combination of single crystal X-ray diffraction, powder X-ray diffraction, Fourier-transform infrared spectroscopy, differential thermal analysis, and thermogravimetric analysis. In contrast, mechanochemical methods, including neat grinding (without solvent) and liquid-assisted grinding (with minimum solvent), enabled selective formation of either a phase pure CC or ICC form. Less polar and nonpolar organic solvents favor the kinetic CC, while polar water promotes formation of the thermodynamically stable ICC. Time-resolved in situ powder X-ray diffraction (TRIS-PXRD) captures the dynamic evolution of solid-state phases and reveals the complete transformation of the CC into ICC under neat grinding or water-assisted conditions. This study highlights the powerful role of mechanochemistry and in situ monitoring in steering solid-state reactivity and offers a sustainable pathway for the targeted and scalable synthesis of pure multicomponent organic materials.
KW - Cocrystal
KW - Synchrotron X-ray powder diffraction
KW - Time-resolved in situ investigation
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641409
DO - https://doi.org/10.1039/D5CE00663E
SN - 1466-8033
SP - 1
EP - 9
PB - Royal Society of Chemistry (RSC)
CY - Cambridge
AN - OPUS4-64140
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Paul, Sagar
A1 - Dolai, Malay
A1 - Nanda Goswami, Juli
A1 - Bhattacharya, Biswajit
A1 - Emmerling, Franziska
A1 - Drew, Michael G. B.
A1 - Chattopadhyay, Shouvik
A1 - Sarkar, Rabi Sankar
A1 - Sunil, Appu
A1 - Novitchi, Ghenadie
A1 - Moreno-Pineda, Eufemio
A1 - Wernsdorfer, Wolfgang
T1 - From strong to weak interaction: Reconciling SQUID and μSQUID-EPR data in anomalous Co(ii) dimers
N2 - Magnetic molecules have been proposed as scaffolds for novel quantum technologies, ranging from quantum sensing and quantum memory to multilevel quantum bits (qudits) and fault-tolerant quantum computation. Integration of magnetic molecules into cutting-edge applications hinges on a deep understanding and tunability of their spin states. To date, the strategic manipulation of the local environment of the ion and careful selection of the magnetic core have enabled the desired tunability and scalability of the spin states. For such goals, however, extracting the anisotropic parameters that dictate the characteristics of the Spin Hamiltonian is challenging, especially for molecules consisting of multiple magnetic cores. We address these challenges by studying two cobalt(II) dinuclear systems, complicated by inherent spin–orbit coupling. We explore the magnetic properties of these systems in two temperature regimes: (i) at sub-Kelvin temperatures employing single crystals at 30 mK using a unique μSQUID-EPR technique that examines the microwave absorption peaks in the magnetisation data and their variation with field angle and frequency; and (ii) in bulk employing convectional SQUID magnetometry above 2 K i.e., χMT(T) and M(H). Unexpectedly, sub-Kelvin temperature investigations reveal a negligible interaction, whereas the SQUID data reveal a much stronger interaction between the Co(II) ions. An understanding of these data is developed based on a strong coupling model and the coupling of two moieties with a spin-effective ground state.
KW - cOBALT(II)-complex
KW - In situ complex formation
KW - Magnetic property
KW - Crystal structure
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641421
DO - https://doi.org/10.1039/D5QI01387A
SN - 2052-1553
SP - 1
EP - 13
PB - Royal Society of Chemistry (RSC)
CY - Cambridge
AN - OPUS4-64142
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Mishra, Rajesh K.
A1 - Minussi, F.B.
A1 - Kumari, Priyanka
A1 - Shahi, Rohit R.
A1 - Yadav, R.P.
A1 - Emmerling, Franziska
A1 - Araújo, E.B.
T1 - Effect of sintering temperature on structural, microstructural, and dielectric properties of (Co0.2Fe0.2Ni0.2Al0.2Ti0.2)3O4 multi-cations high entropy oxides
N2 - The study reports the effect of sintering temperature on structural, microstructural, and dielectric properties of (Co0.2Fe0.2Ni0.2Al0.2Ti0.2)3O4 spinel high-entropy oxides (HEOs) synthesized through the solid-state mechanochemistry method. The sintering of the ceramic powders was accomplished at three different temperatures (1000 ◦C, 1100 ◦C, and 1250 ◦C), followed by air quenching. XRD analysis along with Le-Bail refinement confirms that 1100 ◦C and 1250 ◦C sintered oxides comprised of a single cubic spinel phase (Fd3m), while 1000 ◦C sintered oxide contains constituent oxides and a spinel phase. The phase formation of oxides sintered at 1100 ◦C and 1250 ◦C has also been confirmed by Raman spectroscopic analysis. Microstructural analysis revealed that the aggregated particle size increases with the rise in sintering temperature. With the change in sintering temperature, the dielectric behavior of the ceramic changed extensively. The 1100 ◦C sintered ceramic exhibits high frequency-dependent behavior, whereas the 1250 ◦C sintered ceramic yields low frequency-dependent behavior. The 1250 ◦C sintered HEO exhibits low-loss tangent (tan δ = 0.01) with higher dielectric permittivity (εʹ = 44) at high frequency (1 MHz) compared to the 1100 ◦C sintered ceramic and many other conventional dielectrics.
Fractal concept and impedance analysis have been employed to correlate the microstructure-dielectric property relation of (Co0.2Fe0.2Ni0.2Al0.2Ti0.2)3O4 spinel HEOs. The found Hurst exponent values for both different temperature-sintered HEOs are less than 0.5, indicating the anti-persistent behavior. This signifies that the height variations at neighboring pixels are negatively correlated. The present work is of fundamental importance in employing fractal analysis for the first time on spinel HEOs and correlating their properties. It also shows that processing conditions can effectively tailor the dielectric properties of the materials.
KW - Multi-cations high entropy oxide
KW - Mechanochemistry
KW - Spinel structure
KW - Fractal and impedance spectroscopic analysis
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-647584
DO - https://doi.org/10.1016/j.ceramint.2025.09.256
SN - 0272-8842
VL - 51
IS - 27
SP - 55341
EP - 55354
PB - Elsevier Ltd.
AN - OPUS4-64758
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Karafiludis, Stephanos
A1 - Standl, Jacob
A1 - Ryll, Tom W.
A1 - Schwab, Alexander
A1 - Prinz, Carsten
A1 - Wolf, Jakob B.
A1 - Kruschwitz, Sabine
A1 - Emmerling, Franziska
A1 - Völker, Christoph
A1 - Stawski, Tomasz M.
T1 - High-Entropy Phosphate Synthesis: Advancements through Automation and Sequential Learning Optimization
N2 - Transition metal phosphates (TMPs) are extensively explored for electrochemical and catalytical applications due to their structural versatility and chemical stability. Within this material class, novel high-entropy metal phosphates (HEMPs)─containing multiple transition metals combined into a single-phase structure─are particularly promising, as their compositional complexity can significantly enhance functional properties. However, the discovery of suitable HEMP compositions is hindered by the vast compositional design space and complex or very specific synthesis conditions. Here, we present a data-driven strategy combining automated wet-chemical synthesis with a Sequential Learning App for Materials Discovery (SLAMD) framework (Random Forest regression model) to efficiently explore and optimize HEMP compositions. Using a limited set of initial experiments, we identified multimetal compositions in a single-phase crystalline solid. The model successfully predicted a novel Co0.3Ni0.3Fe0.2Cd0.1Mn0.1 phosphate octahydrate phase, validated experimentally, demonstrating the effectiveness of the machine learning approach. This work highlights the potential of integrating automated synthesis platforms with data-driven algorithms to accelerate the discovery of high-entropy materials, offering an efficient design pathway to advanced functional materials.
KW - Metal phosphates
KW - High entropy
KW - Sequential learning
KW - Automated synthesis
KW - MAP
KW - Random forest
KW - Machine learning
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641554
DO - https://doi.org/10.1021/acs.cgd.5c00549
SN - 1528-7483
VL - 25
IS - 19
SP - 7989
EP - 8001
PB - American Chemical Society (ACS)
CY - Washington, DC
AN - OPUS4-64155
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Batteas, James
A1 - Blank, Kerstin G.
A1 - Colacino, Evelina
A1 - Emmerling, Franziska
A1 - Friščić, Tomislav
A1 - Mack, James
A1 - Moore, Jeffrey
A1 - Rivas, Maria Elena
A1 - Tysoe, Wilfred
T1 - Moving mechanochemistry forward
N2 - Arguably mechanochemistry is one of the oldest, and at the same time one of the newest, areas of chemistry. One of the oldest, because it has been theorized that early hominids were able to develop rapidly due to their ability to heat and mechanically process their food to make it easier to digest. Old, because the ancient Greeks knew that mechanically activating stones (consisting of cinnabar) with vinegar in a copper pestle and mortar caused them to convert into mercury. We might be forgiven for thinking that this could have led our alchemical forbears to wonder if there were other stones that might also be persuaded to convert into gold. Early chemical luminaries such as Michael Faraday and Wilhelm Röntgen dabbled in mechanochemistry. However, in the late 19th and early 20th centuries, the field developed separately in many areas. Perhaps most significantly, synthetic chemists realized that reactions could be carried out with surprisingly high yields and selectivities by shaking them in a ball mill, and that they could even make novel compounds that their colleagues just using heat were not able to. Physicists were mechanically rearranging atoms into new configurations (i.e., doing chemistry) using exotic means such as atomic force microscope tips and optical tweezers. Scientists and engineers studying the formation of lubricious and anti-wear films realized that they were mechanochemically formed. Biochemists found molecular motor proteins, such as myosin and kinesin, that were able to convert chemical energy into motion or, vice versa, mechanical energy into the biochemical energy storage molecule adenosine triphosphate. In 2023, this confluence of advances convinced the Royal Society of Chemistry that the time was ripe to establish a new journal dedicated to the field of mechanochemistry. It is rare that a journal has the privilege of helping to create a new sub-branch of chemistry but, having done so, it has the obligation of helping to define the field and, optimistically, suggesting how the field might develop. This editorial has two major goals. The first is to bring to the attention of the scientific community the challenges faced by the field to set people thinking about how they might contribute and, second, to form the basis for more thorough discussions in the future. The sub-topics below outline current thoughts brought forward from members of our editorial board. We lay out areas and topics here with the intent of establishing a new editorial series, which we invite the community to contribute to, and outline topics and hopefully lay out challenges, which will enable us as a community to come together to move mechanochemistry forward.
KW - Mechanochemistry
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-646086
DO - https://doi.org/10.1039/d4mr90021a
SN - 2976-8683
VL - 2
IS - 1
SP - 10
EP - 19
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64608
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Ferreira, Daniela R.
A1 - Portet, Anaïs
A1 - Alves, Paula C.
A1 - Rijo, Patrícia
A1 - Gomes, Clara S. B.
A1 - Duarte, M. Teresa
A1 - Halasz, Ivan
A1 - Colacino, Evelina
A1 - Emmerling, Franziska
A1 - André, Vânia
T1 - Modulating the crystalline forms of silver–sulfadiazine complexes by mechanochemistry
N2 - Mechanochemical synthesis of pharmaceutical compounds has gained significant attention due to its potential to overcome traditional synthetic challenges while offering the possibility of improving the physicochemical properties of drugs. This study delves into the mechanochemical synthesis of silver sulfadiazine (AgSD) coordination compounds, obtained under different mechanochemical stress and processing conditions. The aim of this work was to investigate the influence of mechanochemical conditions on the selectivity in the preparation of AgSD coordination compounds. Through a series of experiments, we demonstrate the successful synthesis of two different AgSD coordination networks, using high-energy ball milling. By strategically manipulating the starting materials and milling parameters — including milling time, milling frequency, type of mechanical stress (as determined by different milling devices), and the presence of co-milling agents — we were able to control the product outcome. As a result, we achieved two different forms of silver-sulfadiazine metal frameworks, one of which was not previously disclosed. The crystal structure of the new form, obtained from high resolution PXRD synchrotron data, was compared with the previously known structure of a silver sulfadiazine compound. The in-depth antimicrobial activity systematic study of these AgSD forms on the generic systems showed increased antibacterial activity when compared to sulfadiazine. This research sheds light on the mechanochemical synthesis of silver sulfadiazine complexes. The obtained knowledge may guide the development of novel synthetic strategies for other drug molecules, leading to improved drug performance, stability, and therapeutic outcomes.
KW - Mechanochemistry
KW - Structure solution
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-646099
DO - https://doi.org/10.1039/d5ce00572h
SN - 1466-8033
SP - 1
EP - 12
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64609
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Rodríguez-Sánchez, Noelia
A1 - Prinz, Carsten
A1 - Bienert, Ralf
A1 - Ballesteros, Menta
A1 - Ruiz Salvador, A. Rabdel
A1 - Bhattacharya, Biswajit
A1 - Emmerling, Franziska
T1 - Mechanochemical ZIF-9 formation: in situ analysis and photocatalytic enhancement evaluation
N2 - Efficient treatment of persistent pollutants in wastewater is crucial for sustainable water management and environmental protection. This study addresses this challenge by investigating the mechanochemical synthesis and photocatalytic performance of ZIF-9, a cobalt-based zeolitic imidazolate framework. Using synchrotron-based powder X-ray diffraction, we provide real-time insights into the formation dynamics of ZIF-9 during mechanosynthesis. Our results show that mechanochemically synthesised ZIF-9 exhibits superior photocatalytic activity compared to its solvothermally prepared counterpart, achieving a 2-fold increase in methylene blue degradation rate. This research not only advances our understanding of the synthesis and properties of ZIF-9, but also demonstrates the potential of mechanochemical approaches in the development of high-performance, sustainably produced materials for water treatment and other environmental applications.
KW - MOFs
KW - ZIF
KW - Time-resolved in situ investigation
KW - Photocatalysis synchrotron X-ray powder diffraction
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641416
DO - https://doi.org/10.1039/D4MR00114A
SN - 2976-8683
VL - 2
IS - 1
SP - 116
EP - 126
PB - Royal Society of Chemistry (RSC)
CY - Cambridge
AN - OPUS4-64141
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Lopes, Chrystal
A1 - Casali, Lucia
A1 - Emmerling, Franziska
A1 - Leyssens, Tom
A1 - Dupray, Valérie
A1 - Brandel, Clement
A1 - Cartigny, Yohann
T1 - Efficient racemization of the pharmaceutical compound Levetiracetam using solvent-free mechanochemistry
N2 - We present the racemization of an active pharmaceutical ingredient Levetiracetam using a novel approach. We demonstrate the design of a 100% solvent-free process that proceeds by high energy milling inside a regular mixer mill. The kinetics of the racemization process is drastically improved compared to the solution-based approach and illustrates the tremendous potential of mechanochemistry. In this study, we highlight the importance of mixing efficiency regarding data reproducibility, and we show, in particular, that water contamination has a negative impact on the reaction rate. Moreover, in situ X-ray diffraction gives us first insights into the mechanisms involved in the solid state during the mechanochemical racemization process.
KW - Mechanochemistry
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-646108
DO - https://doi.org/10.1039/d4mr00103f
SN - 2976-8683
VL - 2
IS - 1
SP - 83
EP - 90
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64610
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Pavlidis, Sotirios
A1 - Teutloff, Christian
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Krause, Konstantin B.
A1 - Emmerling, Franziska
A1 - Bittl, Robert
A1 - Abbenseth, Josh
T1 - A Crystalline Bismuth(II) Radical Anion: Synthesis, Characterization, and Reactivity
N2 - AbstractWe report the synthesis of a planarized tris‐amidobismuthane supported by a rigid, bulky NNN pincer ligand, which enforces a T‐shaped geometry at the bismuth center. The Bi(NNN) complex features a low‐lying LUMO with distinct Bi(6p) orbital character as shown by DFT calculations. Cyclic voltammetry reveals a fully reversible one‐electron reduction at E1/2 = –1.85 V versus Fc0/+ in THF. Chemical reduction with KC8 in the presence of 4,7,13,16,21,24‐hexaoxa‐1,10‐diazabicyclo[8.8.8]hexacosane (222‐crypt) enables the isolation of an unprecedented Bi(II) radical anion in high isolated yields. Multi‐frequency EPR, X‐ray absorption spectroscopy and SQUID magnetometry complemented by theoretical calculations confirm localization of the unpaired electron on the bismuth center. Preliminary reactivity studies display radical reactivity as shown by single‐electron transfer chemistry and radical coupling reactions.
KW - Bi(III)
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-644143
DO - https://doi.org/10.1002/anie.202515545
SN - 1433-7851
VL - 64
IS - 49
SP - 1
EP - 6
PB - Wiley VHC-Verlag
AN - OPUS4-64414
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Schmalz, Alina
A1 - Eby, Charles Gaston
A1 - Moss, Caitlin
A1 - Bhattacharya, Biswajit
A1 - Emmerling, Franziska
T1 - Thermally Robust 1D Cu(I) Phosphonate Coordination Polymer Exhibiting Enhanced Proton Conductivity via Humidity‐Driven Pathways
N2 - The development of thermally stable solid-state proton conductors (SSPCs) is crucial for advancing energy-conversion devices such as proton-exchange membrane fuel cells (PEMFCs). In this work, we report the solvothermal synthesis and characterization of a novel, 1D Cu(I) coordination polymer, {Cu(ADP)0.5(BPY)}n (BAM-5), based on anthracenediylphosphonate (H2ADP) and 4,40 -bipyridine (BPY). Single-crystal X-ray diffraction revealed that BAM-5 crystallizes in the triclinic space group P1 and shows a 1D ladder structure connected by the H2ADP and organic BPY linkers, which is assembled into a 2D layer via O−H···O hydrogen bonding interactions between uncoordinated oxygen and the O−H of the phosphonate group. Thermogravimetric and dynamic water sorption analysis demonstrated exceptional thermal robustness of BAM-5 until 230°C and notable water affinity. Proton conductivity measurements found increasing proton conductive properties with increasing temperature and relative humidity.The latter is correlated with the material’s water uptake since the structure itself does not contain any permanent lattice water molecules. A maximum proton conductivity of 6.6 × 10−6 S cm−1 was found at 80°C and 98% RH. To the best of our knowledge, no dense, nonporous 1D coordination polymer without lattice or coordinated solvent molecules has shown comparable proton con� ductivity. The high activation energy suggests a combination of both, a Grotthuss-type proton hopping through the hydrogen� bonded framework, and a vehicular process, in which protons are carried along with absorbed water molecules.
KW - Coordination polymers
KW - Phosphonate ligand
KW - Proton conduction
KW - X-ray diffraction
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-651382
DO - https://doi.org/10.1002/zaac.202500187
SN - 0044-2313
SP - 1
EP - 8
PB - Wiley VHC-Verlag
AN - OPUS4-65138
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Hoque, Maroof Arshadul
A1 - Sommerfeld, Thomas
A1 - Lisec, Jan
A1 - Das, Prasenjit
A1 - Prinz, Carsten
A1 - Heinekamp, Christian
A1 - Stolar, Tomislav
A1 - Etter, Martin
A1 - Rosenberger, David
A1 - George, Janine
A1 - Bhattacharya, Biswajit
A1 - Emmerling, Franziska
T1 - Mechanochemically Synthesized Covalent Organic Framework Effectively Captures PFAS Contaminants
N2 - Per‐ and polyfluoroalkyl substances (PFAS) are persistent environmental contaminants that pose significant health risks, prompting urgent efforts to develop effective removal methods and adsorbers. Covalent organic frameworks (COFs) are metal‐free adsorbers with high stability and tunable porosity. A highly crystalline COF is synthesised mechanochemically using 1,3,5‐tris(4‐aminophenyl)benzene (TAPB) and 1,3,5‐triformylbenzene (TFB). The formation dynamics are monitored in real time with time‐resolved in situ synchrotron X‐ray diffraction. The TAPB‐TFB COF demonstrates good efficiency in eliminating PFAS from water. Perfluorooctanoic acid (PFOA) and perfluorooctanesulfonic acid (PFOS) are effectively extracted, and most of the adsorption occurred within the first 10 min. Additionally, X‐ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, and DFT calculations are employed to elucidate the molecular interactions between PFAS and the COF framework. The rapid and efficient removal of PFAS makes TAPB‐TFB COF a promising material for water treatment applications.
KW - COFs
KW - Ball-milling
KW - PFAS
PY - 2025
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-648712
DO - https://doi.org/10.1002/smll.202509275
SN - 1613-6810
VL - 21
IS - 44
SP - 1
EP - 8
PB - Wiley
CY - Weinheim
AN - OPUS4-64871
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Parthasarathy, Thiyagaraj
A1 - Mishra, Manish Kumar
A1 - Bhattacharya, Biswajit
A1 - Emmerling, Franziska
A1 - Ghosh, Soumyajit
T1 - Simultaneously Mechanically Flexible, Photobending, and Acidochromic Cyanostilbene Molecular Crystals
N2 - Molecular crystals that respond to multiple stimuli are gaining significant attention for their potential in smart materials like actuators and sensors. However, imparting multiple stimuli-responsive properties to a single crystal remains a major challenge. Herein, we report two cyanostilbene derivative-based crystals 1 and 2, with various responses to stimuli such as mechanical stress, light, acid vapors, etc. Both crystals 1 and 2 demonstrated mechanical flexibility and reversible acidochromism. Additionally, crystal 1 also exhibited light-induced photobending, which is ascribed to Z to E photoisomerization. Detailed structure–property correlation was established to unravel distinct mechanical responses. The development of these multitasking crystals may find applications in multitasking actuators, anticounterfeiting materials, and more.
KW - Absorption
KW - Crystals
KW - Mechanical flexiblity
KW - Photoisomerization
PY - 2025
DO - https://doi.org/10.1021/acs.cgd.4c01341
VL - 25
IS - 2
SP - 309
EP - 318
PB - American Chemical Society (ACS)
AN - OPUS4-62568
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Nag, Sayak
A1 - Bhattacharya, Biswajit
A1 - Emmerling, Franziska
A1 - Ghosh, Soumyajit
T1 - Stress and Light-Induced Dual Mechanical Properties of Two 1,3-Dicyanostilbene Derivative Crystals
N2 - Dynamic molecular crystals with multistimuli responses hold immense potential for applications as actuators and smart materials. Here, we report two new 1,3-dicyanostilbene derivative crystals (crystals 1 and 2), which exhibit dual mechanical responses. Both crystals 1 and 2 demonstrate stress-induced mechanical flexibility and light-induced photomechanical bending upon exposure to a 375 nm UV LED. These two distinct mechanical responses are associated with different underlying phenomena and are independent of each other. Mechanical flexibility is attributed to the absence of slip planes and a criss-cross packing arrangement in an isotropic structure, while photomechanical bending is ascribed to the formation of a heterogeneous phase distribution due to Z → E photoisomerization. However, they show thermal reversibility, pointing toward a reversible E → Z back isomerization. This study demonstrates that single molecular crystals combining mechanical flexibility and photomechanical bending can be designed and fabricated for developing multistimuli responsive actuators.
KW - Photoisomerization
KW - Crystal structure
KW - Crystals
KW - Flexibility
KW - Molecules
PY - 2025
DO - https://doi.org/10.1021/acs.cgd.5c00097
SN - 1528-7483
SP - 1
EP - 11
PB - American Chemical Society (ACS)
AN - OPUS4-63267
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Purohit, Akash M
A1 - Patel, Rishi I
A1 - Bhatt, Vidhi
A1 - Mosaffa, Elias
A1 - Bhattacharya, Biswajit
A1 - Manna, Arun K
A1 - Iyer, Bragadish
A1 - Emmerling, Franziska
A1 - Banerjee, Atanu
T1 - Solvent induced ligand transmuted substituted pyrazole housed copper complexes: Synthesis, characterization, DFT and anti-microbial performance
N2 - Pyrazole-based ligand systems 3,5-dimethylpyrazole (L1) and 1-hydroxymethyl-3,5-dimethylpyrazole (L2OH) were synthesized and utilized to form copper complexes in various solvent environments. The ligand L2OH exhibits significant solvent-induced ligand transformation in polar protic solvent. The structural and electronic characteristics of the synthesized complexes were elucidated by X-ray single crystallography, Fourier Transform Infrared (FTIR) and electronic spectroscopy (UV-VIS). Whereas the ligand transformation has been evidenced from FTIR and Nuclear Magnetic Resonance (NMR) spectroscopic techniques. Furthermore, Density Functional Theory (DFT) highlights the pivotal role of solvent effects in modulating ligand transformations and complex formation, contributing to the rational design of metal-based bioactive compounds. Electronic transitions of the metal complexes have been analysed by time-dependent DFT (TD-DFT) calculations. The findings reinforce the significance of transition metal complexes in the development of antimicrobial agents and metallo-pharmaceuticals. The synthesized pyrazole compounds showed 100% inhibition against bacterial strains Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus, and Bacillus subtilis and the yeast Candida albicans at a concentration ranging from 3.9 to 62.5 µg/ml depending upon the strain tested.
KW - Pyrazole derivatives
KW - Antibacterial and antifungal activity
KW - Solvent induced ligand transformation Copper complexes
KW - DFT study
PY - 2025
DO - https://doi.org/10.1016/j.molstruc.2025.143001
SN - 0022-2860
VL - 1345
SP - 1
EP - 12
PB - Elsevier B.V.
AN - OPUS4-63746
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Alić, Jasna
A1 - Schlegel, Moritz-Caspar
A1 - Emmerling, Franziska
A1 - Stolar, Tomislav
T1 - Meeting the UN Sustainable Development Goals with Mechanochemistry
N2 - Chemistry traditionally relies on reactions in solution, but this method is increasingly problematic due to the scale of chemical processes and their economic and environmental impact. Handling residual chemical waste, including solvents, incurs significant costs and environmental pressure. Conversely, novel chemical approaches are needed to address pressing societal issues such as climate change, energy scarcity, food insecurity, and waste pollution. Mechanochemistry, a sustainable chemistry discipline that uses mechanical action to induce chemical reactivity without bulk solvents, is a hot topic in academic research on sustainable and green chemistry. Given its fundamentally different working principles from solution chemistry, mechanochemistry offers more efficient chemical processes and the opportunity to design new chemical reactions. Mechanochemistry has a profound impact on many urgent issues facing our society and it is now necessary to use mechanochemistry to address them. This Minireview aims to provide a guide for using mechanochemistry to meet the United Nations (UN) Sustainable Development Goals (SDGs), thereby contributing to a prosperous society. Detailed analysis shows that mechanochemistry connects with most UN SDGs and offers more cost‐efficiency than other approaches together with a superior environmental performance.
KW - Mechanochemistry
KW - SDGs
PY - 2024
DO - https://doi.org/10.1002/anie.202414745
SP - 1
EP - 3
PB - Wiley
AN - OPUS4-61108
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Nag, Sayak
A1 - Emmerling, Franziska
A1 - Tothadi, Srinu
A1 - Bhattacharya, Biswajit
A1 - Ghosh, Soumyajit
T1 - Distinct photomechanical responses of two new 1,3-dimethylbarbituric acid derivative crystals
N2 - We demonstrate two distinct photomechanical responses (i.e. photomechanical bending and photosalient bursting) of two new 1,3-dimethylbarbituric acid derivative crystals based on tailoring their substituents and the modulation of their spacers.
KW - Crystal engineering
KW - Fexible crystals
PY - 2024
DO - https://doi.org/10.1039/D4CE00233D
SP - 1
EP - 12
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-60141
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Miliūtė, Aistė
A1 - Bustamante, Joana
A1 - Karafiludis, Stephanos
A1 - Zöllner, Moritz
A1 - Eddah, Mustapha
A1 - Emmerling, Franziska
A1 - Mieller, Björn
A1 - George, Janine
A1 - Stawski, Tomasz M.
T1 - Synthesis and phase purity of the negative thermal expansion material ZrV2O7
N2 - Synthesis of pure, homogeneous, and reproducible materials is key for the comprehensive understanding, design, and tailoring of material properties. In this study, we focus on the synthesis of ZrV2O7, a material known for its negative thermal expansion properties. We investigate the influence of solid-state and wet chemistry synthesis methods on the purity and homogeneity of ZrV2O7 samples. Our findings indicate that different synthesis methods significantly impact the material's characteristics. The solid-state reaction provided high-purity material through extended milling time and repeated calcination cycles, while the sol-gel reaction enabled a “near-atomic” level of mixing and, therefore, homogenous phase-pure ZrV2O7. We confirmed purity via X-ray diffraction and Raman spectroscopy, highlighting differences between phase-pure and multiphase ceramics. These analytical techniques allowed us to distinguish subtle differences in the structure of the material. Based on ab initio simulated phonon data, we were able to interpret the Raman spectra and visualise Raman active atom vibrations. We show that phase purity enables the unbiased characterisation of material properties such as negative thermal expansion.
KW - NTE
KW - Sol-gel
KW - Solid-state
KW - Ab-initio
KW - XRD
KW - Raman
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624013
DO - https://doi.org/10.1039/d4tc04095c
SN - 2050-7534
SP - 1
EP - 13
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-62401
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Casali, Lucia
A1 - Carta, Maria
A1 - Michalchuk, Adam
A1 - Delogu, Francesco
A1 - Emmerling, Franziska
T1 - Kinetics of the mechanically induced ibuprofen–nicotinamide co-crystal formation by in situ X-ray diffraction
N2 - Mechanochemistry is drawing attention from the pharmaceutical industry given its potential for sustainable material synthesis and manufacture. Scaling mechanochemical processes to industrial level remains a challenge due to an incomplete understanding of their underlying mechanisms. We here show how time-resolved in situ powder X-ray diffraction data, coupled with analytical kinetic modelling, provides a powerful approach to gain mechanistic insight into mechanochemical reactions. By using the ibuprofen–nicotinamide co-crystal mechanosynthesis as a benchmark system, we investigate the behaviour of the solids involved and identify the factors that promote the reaction. As mechanochemical mechanisms become increasingly clear, it promises to become a breakthrough in the industrial preparation of advanced pharmaceuticals.
KW - Mechanochemistry
KW - Kinetics
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608820
DO - https://doi.org/10.1039/D4CP01457J
SN - 1463-9084
VL - 26
SP - 22041
EP - 22048
PB - Royal Society of Chemistry (RSC)
CY - Cambridge
AN - OPUS4-60882
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Gugin, Nikita
A1 - Yusenko, Kirill
A1 - King, Andrew
A1 - Meyer, Klas
A1 - Al-Sabbagh, Dominik
A1 - Villajos Collado, José Antonio
A1 - Emmerling, Franziska
T1 - Lighting up industrial mechanochemistry: Real-time in situ monitoring of reactive extrusion using energy-dispersive X-ray diffraction
N2 - Mechanochemistry is an environmentally friendly synthetic approach that enables the sustainable production of a wide range of chemicals while reducing or eliminating the need for solvents. Reactive extrusion aims to move mechanochemistry from its conventional gram-scale batch reactions, typically performed in laboratory ball mills, to a continuous, large-scale process. Meeting this challenge requires in situ monitoring techniques to gain insights into reactive extrusion and its underlying processes. While the effectiveness of in situ Raman spectroscopy in providing molecular-level information has been demonstrated, our study uses energy-dispersive X-ray diffraction to monitor reactive extrusion in real time at the crystalline level. Our results provide previously unavailable control over the reactive extrusion process, promoting its perception as an industrially feasible green alternative to traditional solvent-based syntheses.
KW - Mechanochemistry
KW - Reactive extrusion
KW - Green chemistry
KW - In situ studies
KW - Time-resolved in situ
KW - TRIS
KW - Synchrotron radiation
KW - Scalable synthesis
KW - Solid-state reactions
KW - Reaction mechanisms
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613969
DO - https://doi.org/10.1016/j.chempr.2024.07.033
VL - 10
IS - 11
SP - 1
EP - 16
PB - Elsevier B.V.
AN - OPUS4-61396
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Stawski, Tomasz
A1 - Karafiludis, Stephanos
A1 - Pimentel, Carlos
A1 - Montes-Hernández, German
A1 - Kochovski, Zdravko
A1 - Bienert, Ralf
A1 - Weimann, Karin
A1 - Emmerling, Franziska
A1 - Scoppola, Ernesto
A1 - Van Driessche, Alexander E.S.
T1 - Solution-driven processing of calcium sulfate: The mechanism of the reversible transformation of gypsum to bassanite in brines
N2 - Here, we show that calcium sulfate dihydrate (gypsum) can be directly, rapidly and reversibly converted to calcium sulfate hemihydrate (bassanite) in high salinity solutions (brines). The optimum conditions for the efficient production of bassanite in a short time (<5 min) involve the use of brines with c(NaCl) > 4 M and maintaining a temperature, T > 80 °C. When the solution containing bassanite crystals is cooled down to around room temperature, eventually gypsum is formed. When the temperature is raised again to T > 80 °C, bassanite is rapidly re-precipitated. This contrasts with the better-known behaviour of the bassanite phase in low-salt environments. In low-salinity aqueous solutions, bassanite is considered to be metastable with respect to gypsum and anhydrite, and therefore gypsum-to-bassanite conversion does not occur in pure water. Interestingly, the high-salinity transformation of gypsum-to-bassanite has been reported by many authors and used in practice for several decades, although its very occurrence actually contradicts numerical thermodynamic predictions regarding solubility of calcium sulfate phases. By following the evolution of crystalline phases with in situ and time-resolved X-ray diffraction/scattering and Raman spectroscopy, we demonstrated that the phase stability in brines at elevated temperatures was inaccurately represented in the thermodynamic databases. Most notably for c(NaCl) > 4 M, and T > 80 °C gypsum becomes readily more soluble than bassanite, which induces the direct precipitation of the latter from gypsum. The fact that these transformations are controlled by the solution provides extensive opportunities for precise manipulation of crystal formation. Our experiments confirmed that bassanite remained the sole crystalline phase for many hours before reverting into gypsum. This property is extremely advantageous for practical processing and efficient crystal extraction in industrial scenarios.
KW - Industrial and Manufacturing Engineering
KW - Strategy and Management
KW - General Environmental Science
KW - Renewable Energy, Sustainability and the Environment
KW - Building and Construction
KW - Calcium sulfate
KW - Gypsum
KW - Bassanite
KW - Scattering
KW - Raman
KW - In situ
KW - Synchrotron
KW - BESSY
KW - MySpot
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594698
UR - https://www.sciencedirect.com/science/article/pii/S0959652624004591#appsec1
DO - https://doi.org/10.1016/j.jclepro.2024.141012
SN - 0959-6526
VL - 440
SP - 1
EP - 12
PB - Elsevier B.V.
AN - OPUS4-59469
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Zuffa, Caterina
A1 - Cappuccino, Chiara
A1 - Casali, Lucia
A1 - Emmerling, Franziska
A1 - Maini, Lucia
T1 - Liquid reagents are not enough for liquid assisted grinding in the synthesis of [(AgBr)(n-pica)]n
N2 - This study investigates the mechanochemical reactions between AgBr 3-picolylamine and 4-picolylamine. The use of different stoichiometry ratios of the reagents allows [(AgBr)(n-pica)]n and [(AgBr)2(n-pica)]n to be obtained, and we report the new structures of [(AgBr)2(3-pica)]n and [(AgBr)2(4-pica)]n which are characterized by the presence of the following: (a) infinite inorganic chains, (b) silver atom coordinated only by bromide atoms and (c) argentophilic interactions. Furthermore, we studied the interconversion of [(AgBr)(n-pica)]n/[(AgBr)2(n-pica)]n by mechanochemical and thermal properties. The in situ experiments suggest that [(AgBr)(3-pica)]n is kinetically favoured while [(AgBr)2(3-pica)]n is converted into [(AgBr)(3-pica)]n only with a high excess of the ligand. Finally, the liquid nature of the ligands is not sufficient to assist the grinding process, and the complete reaction is observed with the addition of a small quantity of acetonitrile.
KW - Mechanochemistry
KW - Complex
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594755
DO - https://doi.org/10.1039/d3cp04791a
SN - 1463-9076
SP - 1
EP - 10
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-59475
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Heinekamp, Christian
A1 - Kneiske, Sönke
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Ahrens, Mike
A1 - Braun, Thomas
A1 - Emmerling, Franziska
T1 - A fluorolytic sol-gel route to access an amorphous Zr fluoride catalyst: A useful tool for C-F bond activation
N2 - A route to a ZrF4 catalyst active in room temperature Friedel–Crafts and dehydrofluorination reactions was developed via a fluorolytic sol–gel route, which was followed by a postfluorination step using a stream of CHClF2. The behaviour of different Zr(IV) precursors in a sol–gel reaction with anhydrous isopropanol/HF solution was investigated. The subsequent post-fluorination step was optimised in its temperature ramp and confirmed the necessity of a fluorination of the generated xerogels to obtain catalytic activity. The process is discussed in the context of the analysis of the materials using Brunauer–Emmett–Teller analysis (BET), powder X-ray diffraction (XRD), infrared spectroscopy (IR), thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The local structure of the amorphous catalyst was elucidated by extended X-ray absorption fine structure spectroscopy (EXAFS).
KW - Catalysis
KW - Heterogeneous catalysis
KW - C-F bond activation
KW - Postfluorination
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593433
DO - https://doi.org/10.1039/D3CY01439H
SN - 2044-4761
SP - 1
EP - 8
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-59343
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Macchietti, Laura
A1 - Casali, Lucia
A1 - Emmerling, Franziska
A1 - Braga, Dario
A1 - Grepioni, Fabrizia
T1 - Deriving kinetic insights from mechanochemically synthesized compounds using multivariate analysis (MCR-ALS) of powder X-ray diffraction data
N2 - Kinetics information on the progress of the mechanochemical reactions is key to their understanding and subsequent scale-up. For crystalline materials, the most robust and tested method for obtaining kinetic data is the Quantitative Phase Analysis (QPA) via Rietveld refinement. In this work, we tested the feasibility of the Multivariate Curve Resolution-Alternating Least Squares (MCR-ALS) method on powder X-ray diffraction (PXRD) data of mechanochemical processes by studying the system theophylline (TP) and malonic acid (MA) in a 1 : 1 stoichiometric ratio at different milling conditions. We have highlighted the strengths and weaknesses of the MCR-ALS method, and we demonstrated why it may be an alternative route to obtain quantitative information on mechanochemical kinetics.
KW - Mechanochemistry
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-646115
DO - https://doi.org/10.1039/d3mr00013c
SN - 2976-8683
VL - 1
IS - 1
SP - 106
EP - 115
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-64611
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Kadri, Lena
A1 - Casali, Lucia
A1 - Emmerling, Franziska
A1 - Tajber, Lidia
T1 - Mechanochemical comparison of ball milling processes for levofloxacin amorphous polymeric systems
N2 - This study aimed to investigate the amorphization capabilities of levofloxacin hemihydrate (LVXh), a fluoroquinolone drug, using a polymer excipient, Eudragit® L100 (EL100). Ball milling (BMing) was chosen as the manufacturing process and multiple mill types were utilized for comparison purposes. The product outcomes of each mill were analyzed in detail. The solid-state of the samples produced was comprehensively characterized by Powder X-ray Diffraction (PXRD), In-situ PXRD, Differential Scanning Calorimetry (DSC), Solid-State Fourier Transform Infrared Spectroscopy (FT-IR), and Dynamic Vapor Sorption (DVS). The crystallographic planes of LVXh were investigated by in-situ PXRD to disclose the presence or absence of weak crystallographic plane(s). The mechanism of LVXh:EL100 system formation was discovered as a two-step process, first involving amorphization of LVXh followed by an interaction with EL100, rather than as an instantaneous process. DVS studies of LVXh:EL100 samples showed different stability properties depending on the mill used and % LVXh present. Overall, a more sustainable approach for achieving full amorphization of the fluoroquinolone drug, LVXh, was accomplished, and advancements to the fast-growing world of pharmaceutical mechano- and tribo-chemistry were made.
KW - Levofloxacin
KW - Eudragit® L100
KW - Mechanochemistry
KW - Phase transformation
KW - In situ monitoring
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611129
DO - https://doi.org/10.1016/j.ijpharm.2024.124652
SN - 0378-5173
VL - 665
SP - 1
EP - 16
PB - Elsevier B.V.
AN - OPUS4-61112
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Baláž, Matej
A1 - Birinci, Mustafa
A1 - Şentürk, Kader
A1 - Achimovičová, Marcela
A1 - Baláž, Peter
A1 - Tampubolon, Imelda Octa
A1 - Stolar, Tomislav
A1 - Bienert, Ralf
A1 - Emmerling, Franziska
A1 - Erdemoğlu, Sema
A1 - Sis, Hikmet
A1 - Erdemoğlu, Murat
T1 - Utilizing Taguchi method and in situ X-ray powder diffraction monitoring to determine the influence of mechanical activation conditions on the physico-chemical properties and Al leachability of K-feldspar
N2 - K-feldspar represents an important natural resource of potassium and aluminum. Within the framework of this study, the K-feldspar was mechanically activated in a planetary ball mill under different conditions planned according to 43 Taguchi orthogonal array experimental design. As outputs, specific surface area (SBET), median particle size (d50), amorphization degree of mineral phases , and Al recovery were used. It was found that the initial d50 value of 293 μm could be reduced to 6.7 μm and the SBET value of 4.7 m2/g could be increased up to 32.5 m2/g upon milling. Both microcline KAl3SiO8, and albite NaAl3SiO8 could be almost completely amorphized, whereas quartz SiO2 still maintained some crystallinity even under the most intensive conditions. Increasing SBET and decreasing the d50 values did not lead to a significant improvement in Al leach recovery, whereas a clear relationship between the amorphization of microcline and the recovered aluminum was found. Analysis of Variance (ANOVA) showed that increasing ball-to-powder ratio is the most beneficial for the improvement in Al recovery. In situ powder X-ray diffraction monitoring performed in an oscillation ball mill under synchrotron irradiation has shown very rapid amorphization of microcline phase at the beginning. However, amorphization of microcline was only partial after two hours of the treatment in this mill, apart from almost complete process in the planetary ball mill. In the end, regressions for the calculation of Al recovery by knowing the values of input parameters were calculated. In general, by just using mechanical activation without the subsequent roasting process that is commonly used to boost metal recoveries, it was possible to quantitatively recover aluminum from K-feldspar.
KW - Mechanochemistry
KW - Mechanical activation
KW - Design of experiments
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611059
DO - https://doi.org/10.1016/j.jmrt.2024.08.156
SN - 2238-7854
VL - 32
SP - 3886
EP - 3895
PB - Elsevier B.V.
AN - OPUS4-61105
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Cakir, Cafer Tufan
A1 - Bogoclu, Can
A1 - Emmerling, Franziska
A1 - Streli, Christina
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Radtke, Martin
T1 - Machine learning for efficient grazing-exit x-ray absorption near edge structure spectroscopy analysis: Bayesian optimization approach
N2 - In materials science, traditional techniques for analyzing layered structures are essential for obtaining information about local structure, electronic properties and chemical states. While valuable, these methods often require high vacuum environments and have limited depth profiling capabilities. The grazing exit x-ray absorption near-edge structure (GE-XANES) technique addresses these limitations by providing depth-resolved insight at ambient conditions, facilitating in situ material analysis without special sample preparation. However, GE-XANES is limited by long data acquisition times, which hinders its practicality for various applications. To overcome this, we have incorporated Bayesian optimization (BO) into the GE-XANES data acquisition process. This innovative approach potentially reduces measurement time by a factor of 50. We have used a standard GE-XANES experiment, which serve as reference, to validate the effectiveness and accuracy of the BO-informed experimental setup. Our results show that this optimized approach maintains data quality while significantly improving efficiency, making GE-XANES more accessible to a wider range of materials science applications.
KW - Machine Learning
KW - GE-XANES
KW - Bayesian Optimization
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-603955
DO - https://doi.org/10.1088/2632-2153/ad4253
VL - 5
IS - 2
SP - 1
EP - 12
PB - IOP Publishing
AN - OPUS4-60395
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Coburger, Peter
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Emmerling, Franziska
A1 - Abbenseth, Josh
T1 - Combining geometric constraint and redox non-innocence within an ambiphilic PBiP pincer ligand
N2 - The first pincer ligand featuring a strictly T-shaped pnictogen donor moiety was synthesised. The PBiP ligand's redox activity facilitates unprecedented ambiphilic bonding of the Bi centre with transition metals through the Bi(6p) orbital.
KW - EXAFS
KW - Pincer Ligand
KW - Group 15 metals
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611113
DO - https://doi.org/10.1039/D4SC00197D
SN - 2041-6520
SP - 1
EP - 8
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-61111
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Schlögl, Johanna
A1 - Goldammer, Ole
A1 - Bader, Julia
A1 - Emmerling, Franziska
A1 - Riedel, Sebastian
T1 - Introducing AFS ([Al(SO3F)3]x) – a thermally stable, readily available, and catalytically active solid Lewis superacid
N2 - This paper introduces the thermally stable, solid Lewis superacid aluminium tris(fluorosulfate) (AFS), that is easy-to-synthesize from commercially available starting materials. Its applicability, e.g. in catalytic C–F bond activations, is shown.
KW - Lewis Acid
KW - C-F activation
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601001
DO - https://doi.org/10.1039/D4SC01753F
SN - 2041-6520
SP - 1
EP - 7
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-60100
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Senges, Gene
A1 - de Oliveira Guilherme Buzanich, Ana
A1 - Lindič, Tilen
A1 - Gully, Tyler A.
A1 - Winter, Marlon
A1 - Radtke, Martin
A1 - Röder, Bettina
A1 - Steinhauer, Simon
A1 - Paulus, Beate
A1 - Emmerling, Franziska
A1 - Riedel, Sebastian
T1 - Unravelling highly oxidized nickel centers in the anodic black film formed during the Simons process by in situ X-ray absorption near edge structure spectroscopy
N2 - The electrofluorination after Simons has been used for the last century to produce everyday life materials. An in situ XANES investigation of the controversially debated black film apparent in the Simons process revealed high-valent nickel centers.
KW - Synchrotron
KW - BAMline
KW - XANES
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608366
DO - https://doi.org/10.1039/d3sc06081k
SN - 2041-6520
VL - 15
IS - 12
SP - 4504
EP - 4509
PB - Royal Society of Chemistry (RSC)
AN - OPUS4-60836
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Das, Prasenjit
A1 - Chakraborty, Gouri
A1 - Friese, Nico
A1 - Roeser, Jérôme
A1 - Prinz, Carsten
A1 - Emmerling, Franziska
A1 - Schmidt, Johannes
A1 - Thomas, Arne
T1 - Heteropolyaromatic Covalent Organic Frameworks via One-Pot Multicomponent Reactions
N2 - Multicomponent reactions (MCRs) offer a platform to create different chemical structures and linkages for highly stable covalent organic frameworks (COFs). As an illustrative example, the multicomponent Povarov reaction generates 2,4-phenylquinoline from aldehydes and amines in the presence of electron-rich alkenes. In this study, we introduce a new domino reaction to generate unprecedented 2,3-phenylquinoline COFs in the presence of epoxystyrene. This work thus presents, for the first time, structural isomeric COFs produced by multicomponent domino and Povarov reactions. Furthermore, 2,3-phenylquinolines can undergo a Scholl reaction to form extended aromatic linkages. With this approach, we synthesize two thermally and chemically stable MCR-COFs and two heteropolyaromatic COFs using both domino and in situ domino and Scholl reactions. The structure and properties of these COFs are compared with the corresponding 2,4-phenylquinoline-linked COF and imine-COF, and their activity toward benzene and cyclohexane sorption and separation is investigated. The position of the pendant phenyl groups within the COF pore plays a crucial role in facilitating the industrially important sorption and separation of benzene over cyclohexane. This study opens a new avenue to construct heteropolyaromatic COFs via MCR reactions.
KW - COF
PY - 2024
UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-604038
DO - https://doi.org/10.1021/jacs.4c02551
SP - 1
EP - 9
PB - American Chemical Society (ACS)
AN - OPUS4-60403
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -
TY - JOUR
A1 - Pakrashy, Sourav
A1 - Chakraborty, Souvik
A1 - Manna, Sounik
A1 - Nanda Goswami, Juli
A1 - Bhattacharya, Biswajit
A1 - Emmerling, Franziska
A1 - Mandal, Jishu
A1 - Misra, Sourav
A1 - Maiti Choudhury, Sujata
A1 - Okla, Mohammad K.
A1 - Bose, Adity
A1 - Maurya, Pawan Kumar
A1 - Majhi, Anjoy
A1 - Dolai, Malay
T1 - Inhibition of Human Colorectal Cancer by a Natural Product 7-Acetylhorminone and Interactions with BSA/HSA: Multispectral Analysis and In Silico and In Vitro Studies
N2 - We have semi-synthesized a natural product 7-acetylhorminone from crude extract of Premna obtusifolia (Indian headache tree), which is active against colorectal cancer after probation through computational screening methods as it passed through the set parameters of pharmacokinetics (most important nonblood–brain barrier permeant) and drug likeliness (e.g., Lipinski’s, Ghose’s, Veber’s rule) which most other phytoconstituents failed to pass combined with docking with EGFR protein which is highly upregulated in the colorectal carcinoma cell. The structure of 7-acetylhorminone was confirmed by single crystal X-ray diffraction studies and 1H NMR, 13C NMR, and COSY studies. To validate the theoretical studies, first, in vitro experiments were carried out against human colorectal carcinoma cell lines (HCT116) which revealed the potent cytotoxic efficacy of 7-acetylhorminone and verified preliminary investigation. Second, the drugability of 7-acetylhorminone interaction with serum albumin proteins (HSA and BSA) is evaluated both theoretically and experimentally via steady-state fluorescence spectroscopic studies, circular dichroism, isothermal titration calorimetry, and molecular docking. In summary, this study reveals the applicability of 7-acetylhorminone as a potent drug candidate or as a combinatorial drug against colorectal cancer.
KW - Molecular docking
KW - In situ synthesis
KW - ADMET
PY - 2024
DO - https://doi.org/10.1021/acsabm.4c00335
VL - 7
IS - 5
SP - 3414
EP - 3430
PB - American Chemical Society (ACS)
AN - OPUS4-61114
LA - eng
AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany
ER -