All materials listed below were of research grade or a spectro grade in the highest purity available and were generally used without purification except 2-pyridinecarboxaldehyde, which was distilled, and acrylonitrile, which was passed through a plug of basic alumina. 1H and proton-decoupled 13C NMR were obtained using a Varian Mercury 400 MHz NMR instrument, and chemical shifts are reported in ppm relative to the deuterated solvent used. Elemental analysis was performed by Atlantic Microlabs (Atlanta, GA, USA). Mass spectral data were obtained on a Bruker AmaZon SL ion trap LC/MS (Northwestern University). X-ray crystallography was performed on a Bruker APEX-II CCD Diffractometer (UC San Diego). Potentiometric titrations were performed using a 785 DMP Titrino equipped with an Accumet double injection pH electrode and thermally regulated titration vessel. Formation-constant data were evaluated using the Hyperquad2008 program suite [28 ]. The fluorescence spectra were recorded using a Cary Eclipse fluorescence spectrophotometer with 3 cm3 quartz cuvette (1 cm pathlength).
Caution! Perchlorates of metal complex cations have been known to explode. No explosions occurred during this work.
Caution! Perchlorates of metal complex cations have been known to explode. No explosions occurred during this work.