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Bottom‐up chemical synthesis to construct intricate molecules has been a profound challenge. An effective approach is to utilize organic ligands and metal ions, but the formation of a single product among other possible candidates was difficult for dissymmetric structures. We now synthesize single isomeric complexes with dissymmetric structures using the mismatch in the coordination valences of macrocyclic homooligomers and metal ions. A series of amide‐cyclodextrin derivatives possessing multiple 2,2´‐bipyridyl (bpy) groups forms mononuclear complexes whose specific three bpy groups are linked with the fac‐Λ configuration. The intermolecular coordination of the β‐cyclodextrin metal complex produces a dissymmetric cyclodextrin trimer as a s.
A strategy for the formation of antimony−carbon bond was developed by nickel‐catalyzed cross‐coupling of halostibines. This method has been applied to the synthesis of various triaryl‐ and diarylalkylstibines from the corresponding cyclic and acyclic halostibines. This protocol showed a wide substrate scope (72 examples) and was compatible to a wide range of functional groups such as aldehyde, ketone, alkene, alkyne, haloarenes (F, Cl, Br, I), and heteroarenes. A successful synthesis of arylated stibine 3a in a scale of 34.77 g demonstrates high synthetic potential of this transformation. The formed stibines (R 3 Sb) were then used for the palladium‐catalyzed carbon−carbon bond forming reaction with aryl boronic acids [R−B(OH) 2 ], giving b.
Lithium‐ion batteries are regarded as the leading contenders in energy storage devices. However, the batteries with routine carbonate electrolytes cannot exhibit satisfactory fast‐charging performance and lithium plating is widely observed at low temperatures. Herein we demonstrate that a localized high‐concentration electrolyte consisting of 1.5 M lithium bis(fluorosulfonyl)imide in dimethoxyethane with bis(2,2,2‐trifluoroethyl) ether as the diluent, enables fast‐charging of working batteries. A uniform and robust solid electrolyte interphase (SEI) can be achieved on graphite surface through the preferential decomposition of anions. The established SEI can significantly inhibit solvent co‐intercalation into graphite and achieve highly reve.
The combination of a chiral copper catalyst and a bifunctional ruthenium pincer complex enables the nonenzymatic dynamic kinetic resolution of acyclic and cyclic benzylic alcohols. The enantioselective Cu‐H‐catalyzed dehydrogenative Si‐O coupling and the rapid transition‐metal‐catalyzed alcohol racemization are perfectly orthogonal. By this, high yields and good levels of enantioselection are achieved. Abstract. A nonenzymatic dynamic kinetic resolution of acyclic and cyclic benzylic alcohols is reported. The approach merges rapid transition‐metal‐catalyzed alcohol racemization and enantioselective Cu‐H‐catalyzed dehydrogenative Si‐O coupling of alcohols and hydrosilanes. The catalytic processes are orthogonal, and the racemization catalyst
Ultrasound (US) produces cavitation‐induced mechanical forces stretching and breaking polymer chains in solution. This type of polymer mechanochemistry is widely used for synthetic polymers, but not biomacromolecules, even though US is biocompatible and commonly used for medical therapy as well as in vivo imaging. The ability to control protein activity by US would thus be a major stepping‐stone for these disciplines. Here, we provide the first examples of selective protein activation and deactivation by means of US. Using GFP as a model system, we engineer US sensitivity into proteins by design. The incorporation of long and highly charged domains enables the efficient transfer of force to the protein structure. We then use this principle
A highly active graphdiyne heterojunction integrated with high‐efficiency photocatalysis is designed and fabricated. This catalyst demonstrates transformative properties on photocatalysis for ammonia synthesis. Such excellent properties are reigned from graphdiyne incorporating Fe site‐specific magnetite resulting in a valence state transition within the catalyst. Our results show the strong advantages of graphdiyne in effectively regulating magnetite activity and coordination environments and also indicate that magnetite can selectively form two different valence tetrahedral coordination Fe and octahedral coordination Fe. The catalysts show remarkable catalytic performance for ammonia synthesis by photocatalysis, indicating transformative
Calculating reaction energy profiles to aid in mechanistic elucidation has long been the domain of the expert computational chemist. Here, we introduce autodE (https://github.com/duartegroup/autodE), an open‐source Python package capable of locating transition states and minima and delivering a full reaction energy profile from 1D or 2D chemical representations. autodE is broadly applicable to study organic and organometallic reaction classes, including addition, substitution, elimination, migratory insertion, oxidative addition and reductive elimination; it accounts for conformational sampling of both minima and TSs, and is compatible with many electronic structure packages. The general applicability of autodE is demonstrated in complex mu.
Mechanoredox is a conceptually new redox system, in which electrons are transferred from distorted piezoelectric materials to trigger organic transformations. In their Communication (DOI: 10.1002/anie.202009844), K. Kubota, H. Ito, and co‐workers describe how the piezoelectric reduction of Umemoto reagents produces a CF3 radical, as represented by the cover picture. Based on this finding, a method for the solid‐state C−H trifluoromethylation of aromatic compounds was developed.
The separation of C 2 H 2 /CO 2 is an essential but challenging process owing to their similar molecular sizes and physical properties. However, it is noteworthy that these two molecules usually exhibit different orientations in the pore channel. Herein, we report an adsorption site selective occupation strategy by taking advantage of differences in orientation to sieving the C 2 H 2 from CO 2 in a judiciously designed amine‐functionalized metal‐organic framework, termed as CPL‐1‐NH 2 . In this material, the incorporation of amino groups not only occupies the adsorption sites of CO 2 molecules and shields the interaction of uncoordinated oxygen atom and CO 2 molecules resulting in a negligible adsorption amount and a decrease in enthalpy of.
The N‐heterocyclic silylene (NHSi) [Ph2P(tBuN)2]SiCl (1), supported by an iminophosphonamide ligand, was obtained from the dehydrochlorination of [Ph2P(tBuN)2]SiHCl2 (2) with LiN(SiMe3)2. NHSi 1 contains an extremely high‐energy HOMO level and consequently displays unique coordination behavior toward Rh(I) complexes. When 1 was treated with 1/4 of an equivalent of [RhCl(cod)]2 (cod = 1,5‐cyclooctadieene), the 14‐electron Y‐shaped bis(chlorosilylene) Rh(I) complex 5 was obtained as dark purple crystals. The reaction of 1 with 1/6 of an equivalent of [RhCl(cod)]2 yielded the cationic tris(silylene)‐Rh(I) complex [6]+·Cl– as red crystals, wherein a two‐coordinated silylene ligand engages in a Si=Rh double bond. A structural analysis of 5 and [
Dehydroalanine (Dha) and dehydrobutyrine (Dhb) display considerable flexibility in a variety of chemical and biological reactions. Natural products containing Dha and/or Dhb residues are often found to possess diverse biological activities. While the ( Z )‐geometry is predominant in nature, only a handful of metabolites containing ( E )‐Dhb have been found thus far. Here we report discovery of a new antimicrobial peptide, albopeptide, through NMR analysis and chemical synthesis, which contains two contiguous unsaturated residues, Dha‐( E )‐Dhb. It displays narrow‐spectrum activity against vancomycin‐resistant Enterococcus faecium. In vitro biochemical assays show that albopeptide originates from a noncanonical NRPS pathway, featured with de.
Simple synthetic routes for heteroatom‐containing polycyclic aromatic hydrocarbons (H‐PAHs) with alkyl and aryl substitution were demonstrated. Three H‐PAHs including heteroatom containing rubicenes (H‐rubicenes), angular‐benzothiophenes (ABTs), and indenothiophene (IDTs) were successfully synthesized through two key steps including polysubstituted olefins formation and cyclization. Specifically, ABT and H‐rubicenes were comprehensively investigated by single‐crystal X‐ray diffraction, NMR, UV‐vis absorption, cyclic voltammetry, transient absorption and single crystal OFET measurements.
Pt‐based materials are widely used as heterogeneous catalysts, in particular for pollutant removal applications. The nature of the active Pt phase responsible for CO oxidation has long been investigated with a view at designing more efficient formulations. The state of Pt has often been proposed to differ depending on experimental conditions, e.g. metallic Pt poisoned with CO being present at lower temperature before light‐off, while an oxidized Pt surface prevails above light‐off temperature. In stark contrast with all previous reports, we show here that both metallic and oxidized Pt are present in similar proportions under reaction conditions at the surface of ca. 1 nm nanoparticles showing high activity at 30 °C. The simultaneous presenc.
Adrenoceptors are ubiquitous and mediate important autonomic functions as well as modulating arousal, cognition and pain on a central level. Understanding these physiological processes and their underlying neural circuits requires manipulating adrenergic neurotransmission with high spatio‐temporal precision. Here we present a first generation of photochromic ligands (adrenoswitches) obtained via azologization of a class of cyclic amidines related to the known ligand clonidine. Their pharmacology, photochromism, bioavailability and lack of toxicity allow for broad biological applications, as demonstrated by controlling locomotion in zebrafish and pupillary responses in mice.
Asymmetric methods that convert racemic starting materials to enantioenriched products are inherently significant in chemical synthesis. Catalytic kinetic resolution (KR) and dynamic kinetic asymmetric transformation (DyKAT) are alternative and complementary avenues to access chiral stereoisomers of both starting materials and reaction products. The development of highly efficient chiral catalytic systems for kinetically controlled processes has therefore been one of the linchpins in asymmetric synthesis. N‐Heterocyclic carbene (NHC)/copper cooperative catalysis has enabled highly efficient KR and DyKAT of racemic N ‐tosylaziridines via [3 + 3] annulation with isatin‐derived enals, leading to highly enantioenriched N ‐tosylaziridine derivat.
We report on the synthesis, structure and physicochemical characterization of the first three examples of neutral palladium‐oxo clusters (POCs). The 16‐palladium(II)‐oxo cluster [Pd 16 O 24 (OH) 8 ((CH 3 ) 2 As) 8 ] ( Pd 16 ) comprises a cyclic palladium‐oxo unit capped by eight dimethylarsinate groups. The chloro‐derivative [Pd 16 Na 2 O 26 (OH) 3 Cl 3 ((CH 3 ) 2 As) 8 ] ( Pd 16 Cl ) was also prepared, which forms a highly stable 3D supramolecular lattice via strong intermolecular interactions. The 24‐palladium(II)‐oxo cluster [Pd 24 O 44 (OH) 8 ((CH 3 ) 2 As) 16 ] ( Pd 24 ) can be considered as a bicapped derivative of Pd 16 with a tetra‐palladium‐oxo unit grafted on either side. The three compounds were fully characterized (i) in the sol.
A racemic and scalable enantioselective total synthesis of (+)‐waihoensene was accomplished. (+)‐Waihoensene belongs to the diterpene natural product family, and features an angular triquinane substructure motif. Its tetracyclic [6.5.5.5]backbone is all‐ cis‐ fused, containing six contiguous stereocenters, four of which are quaternary. These structural features were efficiently installed by means of a diastereoselective radical cyclization, followed by an intramolecular Pauson–Khand reaction, a diastereoselective α‐alkylation, and a diastereoselective 1,4‐addition reaction. Enantioselectivity was introduced at an early stage, by asymmetric palladium catalyzed decarboxylative allylation reaction on gram‐scale.
Deciphering the molecular pictures of the multi‐component and non‐periodic organic‐inorganic interlayer is a grand technical challenge. Here we show that the atomic arrangement of hybrid surface ligands on metal nanoparticles can be precisely quantified through comprehensive characterization of a novel gold cluster, Au 44 ( i Pr 2 ‐bimy) 9 (PA) 6 Br 8 , which features three types of ligands, namely, carbene (1,3‐diisopropylbenzimidazolin‐2‐ylidene, i Pr 2 ‐bimy), alkynyl (phenylacetylide, PA), and halide (Br), respectively. The delicately balanced stereochemical effects and bonding capabilities of the three ligands give rise to peculiar geometrical and electronic structures. Remarkably, despite its complex and highly distorted surface struc.

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