Reactions and manipulations were performed using standard Schlenk techniques or in a nitrogen atmosphere glovebox. HPLC-grade solvents were dried by filtration through activated alumina or distilled under nitrogen over an appropriate drying agent and then used. ESI-MS data for compounds were acquired using a Waters
Micromass Quattro II spectrometer.
1H NMR (500 MHz) and
2H NMR (600 MHz) spectra were referenced to residual solvent relative to TMS.
31P{
1H} NMR (202 and 242 MHz) spectra were referenced to external 85% H
3PO
4. Chemical shifts are reported for room temperature in the
δ scale. FT-IR spectra were recorded on a PerkinElmer
100 FT-IR spectrometer. Crystallographic data for compounds [
1]
0 and [
1]BF
4 were collected using a Siemens SMART diffractometer equipped with a Mo K
α source (
λ = 0.71073 Å).
cis-1,2-Bis(diphenylphosphino)ethylene (dppv) and HBF
4·Et
2O solution were purchased from Aldrich. The compounds Me
2pdtH
2,
56 Fe
2(Me
2pdt)(CO)
6, and Fe
2(Me
2pdt)(CO)
4(dppv) were prepared according to literature procedures.
20 (link),29
Carlson M.R., Gray D.L., Richers C.P., Wang W., Zhao P.H., Rauchfuss T.B., Pelmenschikov V., Pham C.C., Gee L.B., Wang H, & Cramer S.P. (2018). Sterically Stabilized Terminal Hydride of a Diiron Dithiolate. Inorganic chemistry, 57(4), 1988-2001.