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16
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33847065244
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note
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2O for 10 h in 50% aqueous methanol at room temperature and then the solvent was evaporated under reduced pressure. The residues were washed with methanol and dried under vacuum. Metalated peptide conjugates 2-4 were satisfactorily characterized through MALDI ToF and ESI mass spectral analyses.
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19
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33847008454
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note
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EPR spectra were recorded on a Varian spectrometer at X-band frequency and the magnetic field strength was calibrated using DPPH (g = 2.0036). The preformed 1:2 (conjugate/copper and manganese) copper and manganese conjugates 2 and 4 were dissolved in 50% aqueous methanol and EPR spectra were recorded at liquid nitrogen temperature. For pH dependent EPR studies of conjugate 2 (1 mM), the pH was maintained by addition of 10 mM NaOH or HCl. Methanol was added to the aqueous solution to increase the resolution and to avoid aggregation.
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22
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Yao, W.-H.8
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Aronoff-Spencer E., Burns C.S., Avdievich N.I., Gerfen G.J., Peisach J., Antholine W.E., Ball H.L., Cohen F.E., Prusiner S.B., and Millhauser G.L. Biochemistry 39 (2000) 13760
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Chattopadhyay M., Walter E.D., Newell D.J., Jackson P.J., Aronoff-Spencer E., Peisach J., Gerfen G.J., Bennett B., Antholine W.E., and Millhauser G.L. J. Am. Chem. Soc. 127 (2005) 12647
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33847056413
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note
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CD spectra were recorded at 25 °C under a constant flow of nitrogen on a JASCO-810 spectropolarimeter, which was calibrated with an aqueous solution of ammonium d-camphor-10-sulfonate. Experimental measurements were carried out in water (sample concentration was fixed at 0.33 mM, pH 7.5), using a 1 mm path length cuvette between 190 and 400 nm. The spectrum represents an average of 5-8 scans and the CD intensities are expressed in mdeg.
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33
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18344369706
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Burns C.S., Aronoff-Spencer E., Dunham C.M., Lario P., Avdievich N.I., Antholine W.E., Olmstead M.M., Vrielink A., Gerfen G.J., Peisach J., Scott W.G., and Millhauser G.L. Biochemistry 41 (2002) 3991
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Avdievich, N.I.5
Antholine, W.E.6
Olmstead, M.M.7
Vrielink, A.8
Gerfen, G.J.9
Peisach, J.10
Scott, W.G.11
Millhauser, G.L.12
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Barron, L.D.7
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39
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33847071812
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note
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® software, while the data analysis was done with the aid of visual scanning probe microscopy. Conjugates 2-4 (0.33 mM) were incubated in pure water and micrographs were recorded for selected incubation periods. 10 μL of an aqueous solution of each conjugate was transferred onto a freshly cleaved mica surface and uniformly spread with the aid of a spin coater operating at 200-500 rpm (PRS-4000). The sample-coated mica was dried for 30 min at room temperature, followed by AFM imaging.
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40
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Tendler, S.J.B.5
Gazit, E.6
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41
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TGA analysis. Conjugates 1-4 were incubated at 37 °C for 15 days after which the thermal stability of the metallic peptide fibers was determined by thermogravimetric analysis. Thermogravimetric analysis curves were obtained on a Perkin-Elmer Pyris6 thermogravimetry analyzer under zero-grade dry nitrogen atmosphere.
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