Liquid naphthalenes prove to be convenient and versatile solvents for voltammetric measurements, and have revealed a very orderly relationship in electrode potentials for thirty phthalocyanines and porphyrins in nonco-ordinating media a t 150 "C (423 K).
The design of an improved infrared reflection–absorption cell which facilitates the study of redox-active chemical species is described. The modifications to existing cell designs permit (i) the sample to be cooled to temperatures limited by the characteristics of the solvent, (ii) the sample to be maintained under an inert atmosphere, (iii) the study of small (1–2-cm3) volumes of solution, and (iv) the entire optical path to be maintained under vacuum. These features of the cell design facilitate the study of small quantities of compounds which are unstable with respect to reaction with oxygen, moisture, and redox partners. The study of tris-maleonitriledithiolato complexes of chromium in formal oxidation states iv, v, and vi demonstrates the advantages of the cell.
The radical anion species [Os,,C( CO),,]*-and [Os,,H,( CO),,]'-have been prepared by electrochemical and chemical methods (AgBF,-CH,CI, or FeCI,-tetrahydrofuran); as expected they are paramagnetic and exhibit strong signals in their e.s.r. spectra.
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