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11.
Clarke DJ Murray E Hupp T Mackay CL Langridge-Smith PR 《Journal of the American Society for Mass Spectrometry》2011,22(8):1432-1440
Noncovalent protein–ligand and protein–protein complexes are readily detected using electrospray ionization mass spectrometry
(ESI MS). Furthermore, recent reports have demonstrated that careful use of electron capture dissociation (ECD) fragmentation
allows covalent backbone bonds of protein complexes to be dissociated without disruption of noncovalent protein–ligand interactions.
In this way the site of protein–ligand interfaces can be identified. To date, protein–ligand complexes, which have proven
tractable to this technique, have been mediated by ionic electrostatic interactions, i.e., ion pair interactions or salt bridging.
Here we extend this methodology by applying ECD to study a protein–peptide complex that contains no electrostatics interactions.
We analyzed the complex between the 21 kDa p53-inhibitor protein anterior gradient-2 and its hexapeptide binding ligand (PTTIYY).
ECD fragmentation of the 1:1 complex occurs with retention of protein–peptide binding and analysis of the resulting fragments
allows the binding interface to be localized to a C-terminal region between residues 109 and 175. These finding are supported
by a solution-phase competition assay, which implicates the region between residues 108 and 122 within AGR2 as the PTTIYY
binding interface. Our study expands previous findings by demonstrating that top-down ECD mass spectrometry can be used to
determine directly the sites of peptide–protein interfaces. This highlights the growing potential of using ECD and related
top-down fragmentation techniques for interrogation of protein–protein interfaces. 相似文献
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Dr. Ross McLellan Maria A. Palacios Dr. Christine M. Beavers Dr. Simon J. Teat Dr. Stergios Piligkos Prof. Euan K. Brechin Dr. Scott J. Dalgarno 《Chemistry (Weinheim an der Bergstrasse, Germany)》2015,21(7):2804-2812
Methylene‐bridged calix[4]arenes have emerged as extremely versatile ligand supports in the formation of new polymetallic clusters possessing fascinating magnetic properties. Metal ion binding rules established for this building block allow one to partially rationalise the complex assembly process. The ability to covalently link calix[4]arenes at the methylene bridge provides significantly improved control over the introduction of different metal centres to resulting cluster motifs. Clusters assembled from bis‐calix[4]arenes and transition metal ions or 3d‐4f combinations display characteristic features of the analogous calix[4]arene supported clusters, thereby demonstrating an enhanced and rational approach towards the targeted synthesis of complex and challenging structures. 相似文献
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Shaw R Laye RH Jones LF Low DM Talbot-Eeckelaers C Wei Q Milios CJ Teat S Helliwell M Raftery J Evangelisti M Affronte M Collison D Brechin EK McInnes EJ 《Inorganic chemistry》2007,46(12):4968-4978
We report the synthesis, by solvothermal methods, of the tetradecametallic cluster complexes [M14(L)6O6(OMe)18Cl6] (M=FeIII, CrIII) and [V14(L)6O6(OMe)18Cl6-xOx] (L=anion of 1,2,3-triazole or derivative). Crystal structure data are reported for the {M14} complexes [Fe14(C2H2N3)6O6(OMe)18Cl6], [Cr14(bta)6O6(OMe)18Cl6] (btaH=benzotriazole), [V14O6(Me2bta)6(OMe)18Cl6-xOx] [Me2btaH=5,6-Me2-benzotriazole; eight metal sites are VIII, the remainder are disordered between {VIII-Cl}2+ and {VIV=O}2+] and for the distorted [FeIII14O9(OH)(OMe)8(bta)7(MeOH)5(H2O)Cl8] structure that results from non-solvothermal synthetic methods, highlighting the importance of temperature regime in cluster synthesis. Magnetic studies reveal the {Fe14} complexes to have ground state electronic spins of S相似文献
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We have investigated variations in molecularly thin rotaxane films deposited by solvent evaporation, using atomic force microscopy (AFM). Small changes in rotaxane structure result in significant differences in film morphology. The addition of exo-pyridyl moietes to the rotaxane macrocycle results in uniform domains having orientations corresponding to the underlying substrate lattice, while a larger, less symmetric molecule results in a greater lattice mismatch and smaller domain sizes. We have measured differences in film heights both as a function of the solvent of deposition and as a function of surface coverage of rotaxanes. Based on these observations we describe how the use of solvents with higher hydrogen-bond basicity results in films which are more likely to favour sub-molecular motion. 相似文献
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Facile Interchange of 3d and 4f Ions in Single‐Molecule Magnets: Stepwise Assembly of [Mn4], [Mn3Ln] and [Mn2Ln2] Cages within Calix[4]arene Scaffolds 下载免费PDF全文
Dr. Maria A. Palacios Dr. Ross McLellan Dr. Christine M. Beavers Dr. Simon J. Teat Dr. Høgni Weihe Dr. Stergios Piligkos Dr. Scott J. Dalgarno Prof. Euan K. Brechin 《Chemistry (Weinheim an der Bergstrasse, Germany)》2015,21(31):11212-11218
The central MnII ions in a series of calix[4]arene‐stabilised butterflies can be sequentially replaced with LnIII ions, maintaining the structural integrity of the molecule but transforming its magnetic properties. The replacement of MnII for GdIII allows for the examination of the transferability of spin‐Hamiltonian parameters within the family as well as permitting their reliable determination. The introduction of the 4f ions results in weaker intramolecular magnetic exchange, an increase in the number of low‐lying excited states, and an increase in magnetisation relaxation, highlighting the importance of exchange over single‐ion anisotropy for the observation of SMM behaviour in this family of complexes. The presence of the [TMII/III(TBC[4])(OH)(solvent)] metalloligand (TM=transition metal, TBC=p‐tBu‐calix[4]arene) suggests that magnetic calix[n]arene building blocks can be employed to encapsulate a range of different “guests” within structurally robust “hosts”. 相似文献
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