Micromass quattro 2

Unless otherwise stated, reactions were conducted using standard Schlenk techniques, reagents were purchased from conventional sources, and solvents were HPLC grade and purified using an alumina filtration system (Glass Contour, Irvine, CA). ESI-MS data were acquired using a Waters Micromass Quattro II or ZMD spectrometer. Analytical data were acquired using an Exeter Analytical CE-440 elemental analyzer. NMR spectra were acquired with Varian U500 and VXR500 spectrometers. Chemical shifts (ppm) were referenced to residual solvent peaks (for ¹H and ¹³C) or external 85% H₃PO₄ (for ³¹P). Solution IR spectra were recorded on a PerkinElmer Spectrum 100 FTIR spectrometer. Crystallographic data were collected using a Siemens SMART diffractometer equipped with a Mo Kα source (λ = 0.71073 Å) and an Apex II detector. Photolysis employed a Spectroline MB-100 instrument (365 nm). Syntheses of Fe(pdt)(CO)₂(dppv)^{36 (link)} and K[FeCp(CO)₂]³⁷ have been reported. CVs were simulated with the CHI630D package. EPR spectra were recorded on a Varian E-line E-12 Century series X-band CW spectrometer. Spectra were collected at room temperature with a microwave frequency of 9.30 GHz, 1 G modulation, and 20 mW microwave power. EPR spectra were simulated using the program SIMPOW6.³⁸ Samples of [1]⁰ and [H1]⁰ were handled in a glovebox with the exclusion of chlorocarbons.