[NMR paper] Shape and Size Tuning of BiIII-Centered Polyoxopalladates: High Resolution 209Bi NMR and 205/206Bi Radiolabeling for Potential Pharmaceutical Applications.
Shape and Size Tuning of BiIII-Centered Polyoxopalladates: High Resolution 209Bi NMR and 205/206Bi Radiolabeling for Potential Pharmaceutical Applications.
Related ArticlesShape and Size Tuning of BiIII-Centered Polyoxopalladates: High Resolution 209Bi NMR and 205/206Bi Radiolabeling for Potential Pharmaceutical Applications.
Inorg Chem. 2020 Nov 11;:
Authors: Manna P, Szücs D, Csupász T, Fekete A, Szikra D, Lin Z, Gáspár A, Bhattacharya S, Zulaica A, Tóth I, Kortz U
Abstract
We have discovered five bismuth(III)-containing polyoxopalladates (POPs) which were fully characterized by solution and solid-state physicochemical techniques: the cube-shaped [BiPd12O32(AsPh)8]5- (BiPd12AsL), [BiPd12O32(AsC6H4N3)8]5- (BiPd12AsLN), and [BiPd12O32(AsC6H4COO)8]13- (BiPd12AsLC) as well as the star-shaped [BiPd15O40(PO)10H6]11- (BiPd15P) and [BiPd15O40(PPh)10]7- (BiPd15PL), respectively. The organically modified capping groups phenylarsonate, p-azidophenylarsonate, and p-carboxyphenylarsonate were chosen as the azido (-N3) and carboxyl (-COOH) groups open up opportunities to covalently conjugate (via click reaction, amide coupling, etc.) with targeting vectors. The synthesis of p-azidophenylarsonate is reported here for the first time. The effects of the BiIII template and the organoarsonate vs -posphonate capping groups on the resulting POP shape (cube vs star) are discussed. The 209Bi NMR (I = 9/2) spectra of BiPd12AsL, BiPd12AsLN, and BiPd12AsLC revealed narrow peaks (?1/2 ~ 200 Hz) at 5470 ppm with a longitudinal relaxation time in the millisecond range (at 8.46 T). The absence of a quadrupolar relaxation contribution could be attributed to the allocation of BiIII in the highly symmetrical cuboid POP host cage. Similar peaks were absent in the 209Bi-NMR spectra of the star-shaped POPs BiPd15P and BiPd15PL due to the less symmetric coordination environment around the central BiIII ion. Further, 205/206Bi-radiolabeled POPs have been synthesized by incorporating a 205/206BiIII ion in the center of the POP structures. Carrier-free 205/206Bi radioisotopes (as surrogates of ?-emitting 213Bi) were incorporated into the POP host-cage for the preparation of 205/206BiPd12AsL, 205/206BiPd12AsLN, 205/206BiPd12AsLC, and 205/206BiPd15PL, respectively. The radiometal incorporation was complete (>99% radiochemical yield) in 10 min according to radio-thin-layer chromatography. The 205/206BiPd12AsL polyanion was purified by solid-phase extraction. The incubation in rat serum showed the formation of a 205/206BiPd12AsL-protein aggregate.
PMID: 33174740 [PubMed - as supplied by publisher]
[NMR paper] Applications of NMR screening techniques to the pharmaceutical target Checkpoint kinase 1.
Applications of NMR screening techniques to the pharmaceutical target Checkpoint kinase 1.
http://www.bionmr.com//www.ncbi.nlm.nih.gov/corehtml/query/egifs/http:--linkinghub.elsevier.com-ihub-images-PubMedLink.gif Related Articles Applications of NMR screening techniques to the pharmaceutical target Checkpoint kinase 1.
J Pharm Biomed Anal. 2014 May;93:125-35
Authors: Lancelot N, Piotto M, Theret I, Lesur B, Hennig P
Abstract
Ligand screening techniques based on NMR spectroscopy are not as sensitive as other commonly used methods...
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Journal Highlight: On the tuning of high-resolution NMR probes
Journal Highlight: On the tuning of high-resolution NMR probes
http://www.spectroscopynow.com/common/images/thumbnails/14a0562f4b6.jpgThree optimum conditions for the tuning of NMR probes are compared: the conventional tuning optimum, the spin noise tuning optimum and the newly introduced frequency shift tuning optimum.
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12-01-2014 12:17 PM
Quantitative NMR spectroscopy in pharmaceutical applications
Quantitative NMR spectroscopy in pharmaceutical applications
Publication year: 2010
Source:Progress in Nuclear Magnetic Resonance Spectroscopy, Volume 57, Issue 2</br>
Ulrike Holzgrabe</br>
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03-09-2012 09:16 AM
Impact of (15)N R(2)/R(1) Relaxation Restraints on Molecular Size, Shape, and Bond Vector Orientation for NMR Protein Structure Determination with Sparse Distance Restraints.
Impact of (15)N R(2)/R(1) Relaxation Restraints on Molecular Size, Shape, and Bond Vector Orientation for NMR Protein Structure Determination with Sparse Distance Restraints.
Impact of (15)N R(2)/R(1) Relaxation Restraints on Molecular Size, Shape, and Bond Vector Orientation for NMR Protein Structure Determination with Sparse Distance Restraints.
J Am Chem Soc. 2011 Apr 4;
Authors: Ryabov Y, Schwieters CD, Clore GM
(15)N R(2)/R(1) relaxation data contain information on molecular shape and size as well as on bond vector orientations relative to...
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04-06-2011 10:54 AM
Impact of 15N R2/R1 Relaxation Restraints on Molecular Size, Shape, and Bond Vector Orientation for NMR Protein Structure Determination with Sparse Distance Restraints
Impact of 15N R2/R1 Relaxation Restraints on Molecular Size, Shape, and Bond Vector Orientation for NMR Protein Structure Determination with Sparse Distance Restraints
Yaroslav Ryabov, Charles D. Schwieters and G. Marius Clore
http://pubs.acs.org/appl/literatum/publisher/achs/journals/content/jacsat/0/jacsat.ahead-of-print/ja201020c/aop/images/medium/ja-2011-01020c_0002.gif
Journal of the American Chemical Society
DOI: 10.1021/ja201020c
http://feeds.feedburner.com/~ff/acs/jacsat?d=yIl2AUoC8zA
http://feeds.feedburner.com/~r/acs/jacsat/~4/3J1IyCLkQMQ
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Quantitative NMR Spectroscopy in Pharmaceutical Applications
Quantitative NMR Spectroscopy in Pharmaceutical Applications
Publication year: 2010
Source: Progress in Nuclear Magnetic Resonance Spectroscopy, In Press, Accepted Manuscript, Available online 10 May 2010</br>
Ulrike, Holzgrabe</br>
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