The direct electrochemical synthesis of thiolato complexes of copper, silver, and gold; the molecular structure of [Cu(SC₆H₄CH₃-o)(1,10-phenanthroline)]_2•CH₃CN

The direct electrochemical synthesis of thiolato complexes of cobalt and nickel, and the crystal structure of bis(phenylthiolato)bis(1,10-phenanthroline)cobalt(III) perchlorate

“…In previous papers from this laboratory, we have shown that the technique of direct electrochemical synthesis can b e used to prepare thiolato compounds of dl0 metal ions in high yield by a simple one-step room temperature reaction (2)(3)(4)(5)(6). The present paper describes the successful application of this method to the synthesis of various C O ( S R )~ and Ni(SR), compounds, and of a number of neutral adducts.…”

“…This evidence change from red-brown to green when the solution was exposed to does not allow us to identify the reaction unambiguously, but it appears air. In a subsequent experiment, oxygen was bubbled through a to be similar to that observed with C~SC&~(phen), where (C6H5)2S2 solution prepared in the way described above; green crystals deposited and a copper(1) chloride derivative were identified (5 The uv/visible spectrum of 1 had X , , , = 395 nm, E = 2.2 X lo4 mol-' Lcm-I. A prominent feature of the infrared spectrum was a broad strong band at 1070 cm-', identified as v3 of C1O4-.…”

The direct electrochemical synthesis of some metal derivatives of 3-hydroxy-2-methyl-4-pyrone

“…The electrochemical procedures were essentially those described in earlier papers (1)(2)(3)(4)(5)(6)(7)(8)(9)(10)(11). The electrochemical cell was a 100 mL round-bottomed flask with a Schlenk arm containing the solution phase; the sacrificial metal electrode suspended by a platinum wire through the rubber septum was the anode of the cell and a second platinum wire similarly supported was the cathode.…”

“…For copper, the value of 1 .O1 mol F-' indicates the formation of CuL as the primary product, which disproportionates to the element and CuL2 according to [3] 2 CuL -, Cu + CuL2…”

“…A number of papers from this laboratory have demonstrated that the method of direct electrochemical synthesis is a simple, efficient one-step route to the preparation of a wide range of metal complexes, including metal thiolates (1)(2)(3)(4)(5), diphenylphosphides (6), carboxylates (7), catecholates (8,9), and dipyridylamides (10). The method consists simply in the reduction of the selected substrate at an inert platinum cathode in a non-aqueous solution, followed by the oxidation of a sacrificial metal anode.…”