Treatment of the trichlorotin-capped trinuclear nickel cluster, [Ni(dppm)(μ-Cl)(μ-SnCl)], 1, with 4 eq. NaHB(Et) yields a μ-SnH capped trinuclear nickel cluster, [Ni(dppm)(μ-H)(μ-SnH)], 2 [dppm = bis(diphenylphosphino)methane]. Single-crystal X-ray diffraction, nuclear magnetic resonance (NMR) spectroscopy, and computational studies together support that cluster 2 is a divalent tin hydride.
View Article and Find Full Text PDFWe describe the effects of ethanol on the phase behavior of sodium bis(2-ethylhexyl) sulfosuccinate (AOT) in -heptane. Using dynamic light scattering (DLS), molecular dynamics (MD) simulations, and nuclear magnetic resonance (H NMR) spectroscopy, we investigate the aggregation behavior of AOT across a wide range of ethanol/AOT/-heptane compositions. We conclude that reverse micelles do not form at any of the investigated concentrations.
View Article and Find Full Text PDFAnal Bioanal Chem
September 2009
The high sensitivity of silole- and silafluorene-containing polymers for detecting organic nitro, nitrate, and nitramine explosives cannot be solely attributed to favorable analyte-polymer hydrophobic interactions and amplified fluorescence quenching due to delocalization along the polymer chain. The Lewis acidity of silicon in conjugated poly(silafluorene-vinylene)s is shown to be important. This was established by examining the (29)Si NMR chemical shifts (Delta) for the model trimer fragment of the polymer CH(3)-silafluorene-(trans-C(2)H(2))-silafluorene-(trans-C(2)H(2))-silafluorene-CH(3).
View Article and Find Full Text PDFThe first structurally characterized isobutyl-containing aluminoxane compound is presented. The Al10O6iBu16(mu-H)2 (I) cluster is produced from neat octakis-isobutyltetraluminoxane (Al4O2iBu8) at 80 degrees C in 6-8 h followed by slow crystallization. The crystal is triclinic (space group P1) with the molecule lying on an inversion center.
View Article and Find Full Text PDFSolid-state NMR experiments on mechanically aligned bilayer and magnetically aligned bicelle samples demonstrate that membrane proteins undergo rapid rotational diffusion about the normal in phospholipid bilayers. Narrow single-line resonances are observed from 15N labeled sites in the trans-membrane helix of the channel-forming domain of the protein Vpu from HIV-1 in phospholipid bilayers with their normals at angles of 0 degrees, 20 degrees, 40 degrees, and 90 degrees, and bicelles with their normals at angles of 0 degrees and 90 degrees with respect to the direction of the applied magnetic field. This could only occur if the entire polypeptide undergoes rotational diffusion about the bilayer normal.
View Article and Find Full Text PDFHigh-resolution solid-state NMR spectra can be obtained from uniformly (15)N-labeled membrane proteins in magnetically aligned bicelles. Fast uniaxial diffusion about the axis of the bilayer normal results in single-line spectra that contain the orientational information necessary for protein structure determination.
View Article and Find Full Text PDFThe three-dimensional structure of the channel-forming trans-membrane domain of virus protein "u" (Vpu) of HIV-1 was determined by NMR spectroscopy in micelle and bilayer samples. Vpu(2-30+) is a 36-residue polypeptide that consists of residues 2-30 from the N terminus of Vpu and a six-residue "solubility tag" at its C terminus that facilitates the isolation, purification, and sample preparation of this highly hydrophobic minimal channel-forming domain. Nearly all of the resonances in the two-dimensional 1H/15N HSQC spectrum of uniformly 15N labeled Vpu(2-30+) in micelles are superimposable on those from the corresponding residues in the spectrum of full-length Vpu, which indicates that the structure of the trans-membrane domain is not strongly affected by the presence of the cytoplasmic domain at its C terminus.
View Article and Find Full Text PDFThe colorimetric properties of resorcinarene solutions had not been investigated since Baeyer's initial synthesis. We recently reported that solutions containing resorcinarene macrocycles develop color upon heating or standing. In the presence of saccharides, these solutions exhibit significant color changes which are easily seen.
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