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0345442547
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note
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In (15), we stated that when terpy was used, permanganate was not formed. However, we later found that permanganate was being produced in substoichiometric amounts.
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0345011443
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note
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-1); and residuals R(F) = 9.71% for 2501 independent reflections (4° ≤ 2θ ≤ 46°); standard errors in the last decimal place are given in parentheses. In the asymmetric unit, there are two half dimers (each on an inversion center), three nitrate ions, and six water molecules. Despite several attempts at recrystallization, the best crystals that could be obtained were very weak x-ray scatterers (intensity-to-background ratio l/σ = 2.20). All C atoms were refined isotropically to maintain a reasonable data-to-parameter ratio. The H atoms on the aqua ligands and lattice water molecules could not be located from the difference map and were ignored. All other H atoms were treated as idealized contributions. All software sources of the scattering factors are contained in the SHELXTL 5.1 library (Siemens X-ray Diffraction, Madison, WI). The crystal structure data has been deposited at the Cambridge Crystallographic Data Centre (CCDC 113788).
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0345442546
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2-evolution were made with a YSI standard oxygen probe attached to a strip-chart recorder. In a catalytic run, 4 ml of 0.07 M NaClO (pH = 8.6) solution were stirred under the electrode in an airtight system, and an appropriate volume of 1 (1 mM in water at pH = 7) was added from a gastight syringe by means of a small channel along the side of the Teflon-coated holder. Initial rates were calculated for t = 0 to 2 min.
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0344148942
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+ ion, and was equivalent to 40% incorporation into NaOCl.
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41
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0344148941
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note
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UV-vis spectra were taken with an HP 8453 diode array spectrophotometer. For the time-course experiment, 2.5 ml of 200 μM 1 was added to 2.5 ml of 0.5 M NaClO (pH = 8.6); the solution was then mixed and rapidly transferred to a cuvette. For the scans to 280 nm, a 1-mm-pathlength cuvette was used; as with longer pathlengths, the hypochlorite absorbance below 350 nm interfered with the absorbance from the Mn complex.
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42
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0000561889
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0345442545
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note
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2O was isolated and crystallographically characterized (J. Limburg et al., unpublished results), but because 1 is much more soluble, it is more convenient to use for the reactivity studies.
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45
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0345442537
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note
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EPR spectra were recorded on frozen solutions at 10 K with a Varian E-9 X-band spectrometer with a He cryostat at an applied microwave power of 5 mW.
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47
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0344580451
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note
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This work was funded by NIH grant CM32715. The authors thank M.-N. Collomb for communicating experimental data before publication.
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