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Solid-state NMR Spectroscopy of Iodine(I) Complexes.
Chem Asian J
March 2023
University of Jyvaskyla, Department of Chemistry, Jyväskylä, 40014, Finland.
Solid-state NMR has been applied to a series of Barluenga-type iodine(I) [L-I-L]PF (L=pyridine, 4-ethylpyridine, 4-dimethylaminopyridine, isoquinoline) complexes as their hexafluorophosphate salts, as well as their respective non-liquid ligands (L), their precursor silver(I) complexes, and the respective N-methylated pyridinium and quinolinium hexafluorophoshate salts. These results are compared and contrasted to the corresponding solution studies and single-crystal X-ray structures. As the first study of its kind on the solid-state NMR behavior of halogen(I) complexes, practical considerations are also discussed to encourage wider utilization of this technique in the future.
View Article and Find Full Text PDFUtility of Three-Coordinate Silver Complexes Toward the Formation of Iodonium Ions.
Inorg Chem
April 2021
Department of Chemistry, University of Jyvaskyla, Jyväskylä 40014, Finland.
The work herein describes the synthesis of five three-coordinate silver(I) complexes comprising a bidentate ligand L1, either bpy (2,2'-bipyridyl) or bpyMe (4,4'-dimethyl-2,2'-dipyridyl), and a monodentate ligand L2, either mtz (1-methyl-1H-1,2,3-triazole), 4-Etpy (4-ethylpyridine), or 4-DMAP (,-dimethylpyridin-4-amine). Upon reaction of the three-coordinate silver(I) complexes with 0.5 equiv of I, the reactions quantitatively produce a 1:1 pair of complexes of a four-coordinate silver(I) complex [Ag(L1)]PF and a two-coordinate iodonium complex [I(L2)]PF.
View Article and Find Full Text PDFEnergy Migration Processes in Re(I) MLCT Complexes Featuring a Chromophoric Ancillary Ligand.
Inorg Chem
June 2020
Department of Chemistry, North Carolina State University, Raleigh, North Carolina 27695-8204, United States.
We present the synthesis, structural characterization, electronic structure calculations, and ultrafast and supra-nanosecond photophysical properties of a series of five Re(I) bichromophores exhibiting metal to ligand charge transfer (MLCT) excited states based on the general formula -[Re(NN)(CO)(PNI-py)]PF where PNI-py is 4-piperidinyl-1,8-naphthalimidepyridine and NN is a diimine ligand (-), along with their corresponding model chromophores where 4-ethylpyridine was substituted for PNI-py (-). The diimine ligands used include 1,10-phenanthroline (phen, ), 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline (bcp, ), 4,4'-di--butyl-2,2'-bipyridine (dtbb, ), 4,4'-diethyl ester-2,2'-bipyridine (deeb, ), and 2,2'-biquinoline (biq, ). In these metal-organic bichromophores, structural modification of the diimine ligand resulted in substantial changes to the observed energy transfer efficiencies between the two chromophores as a result of the variation in MLCT excited-state energies.
View Article and Find Full Text PDFAdvantageous use of SFC for separation of crude therapeutic peptides and peptide libraries.
J Pharm Biomed Anal
June 2020
ChemPartner Corporation, 280 Utah Avenue, Suite 100, South San Francisco, CA, 94080, United States. Electronic address:
A simple SFC/MS (Supercritical Fluid Chromatography/Mass Spectrometry) method set was developed to effectively screen separations of various crude synthetic peptide products of pharmaceutical interest. Additives to the modifier methanol which were successful for these separations were found to include TFA (trifluoroacetic acid) and ammonia mixed with TFA, each at 0.1 % (v/v) composition in methanol.
View Article and Find Full Text PDFTight Binding of Carboxylate, Phosphonate, and Carbamate Anions to Stoichiometric CdSe Nanocrystals.
J Am Chem Soc
March 2017
Department of Chemistry, Columbia University, 3000 Broadway, MC 3121, New York, New York 10027, United States.
To completely displace the carboxylate surface ligands from cadmium selenide nanocrystals, oleic acid impurities are first removed using dimethylcadmium or diethylzinc. In addition to metal carboxylate and methane coproducts, reactions with CdMe produce surface bound methyl groups (δ = 0.4 ppm, 0.
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