Newton ccd

In a glovebox, 1 mM solutions of (F₈)Fe^II in THF were prepared, transferred to a rR tube, and capped with tight-fitting septa. The sample tubes were placed in a cold bath (dry ice/acetone) and oxygenated using ¹⁶O₂ or ¹⁸O₂ gases. The oxygenated samples were set in a cold bath for 10 min, and to the cold THF solution of [(F₈)Fe^III-(O₂^•−)] (S) was added 1 equiv of CoCp₂ for complex [(F₈)Fe^III-(O₂²⁻)]⁻ (P). Subsequently, 1 equiv of [(LutH⁺)](OTf) was added for complex [(F₈)Fe^III-(OOH)] (HP). The sample tubes were then frozen in liquid N₂ and sealed by flame. Resonance Raman samples were excited at 413 nm using a Coherent I90C-K Kr⁺ ion laser while the sample was immersed in a liquid nitrogen cooled (77 K) EPR finger Dewar (Wilmad). Power was ~2 mW at the sample, which was continuously rotated to minimize photodecomposition. The spectra were recorded using a Spex 1877 CP triple monochromator and detected by an Andor Newton CCD cooled to −80 °C.

All reagents and solvents were of commercially available quality except as noted. Acetone was distilled from Drierite under argon atmosphere. [(MeAN)Cu^I](BAr^F) (BAr^F: B(C₆F₅)₄⁻) was synthesized as previously described.^{24 (link)} Sodium phenolates were obtained using a synthetic method similar to previous results.^{23 (link)} All UV–vis measurements were carried out using a Hewlett-Packard 8453 diode array spectrophotometer with a 10 mm quartz cell. The spectrometer was equipped with HP Chemstation software and a Unisoku cryostat for low temperature experiments. ¹H NMR spectra were recorded on a Bruker 400 instrument. Resonance Raman (rR) samples were excited using a Coherent I90C–K Kr⁺ ion laser at 413.1 or 568.2 nm while the sample was immersed in a liquid-nitrogen-cooled (77 K) EPR finger dewar (Wilmad). Power was ~20 mW at the sample for the 413.1 nm line and ~130 mW at 568.2 nm. Data were recorded while rotating the sample to minimize photodecomposition. The spectra were recorded using a Spex 1877 CP triple monochromator with 600, 1200, or 2400 grooves/mm holographic spectrograph grating and detected by an Andor Newton CCD cooled to −80 °C (413.1 nm) or an Andor IDus CCD cooled to −80 °C (568.2 nm). Spectra were calibrated on the energy axis to toluene at room temperature.