The homoleptic tetraarylaurate anion, Au(C6Cl5)(4)(-), which has never been prepared via traditional chemical methods, has been synthesized by use of an electrochemical technique and crystallized in situ with the bis(ethylenedithio)tetrathiafulvalene tetrathiafulvalene (BEDT-TTF, or ET) electron-donor molecule. This salt, (C10H8S8)Au(C6Cl5)(4), crystallizes having the monoclinic space group P2(1)/c, with a = 14.7835(9) Angstrom, b = 20.2270(12) Angstrom, c = 16.7303(10) Angstrom, beta = 101.396(1)degrees, Z = 4. The crystal structure of this (ET)Au(C6Cl5)(4) salt contains the Au(C6Cl5)(4)(-) anion in an essentially square-planar coordination with the pentachlorophenyl groups arranged in a propeller-like D-4 symmetry, consistent with the formal oxidation state +3 of the central metal atom. The ET+ cations are completely surrounded by the pentachlorophenyl rings of the anions, thereby precluding the formation of a S...S network with concomitant conducting properties. Analysis of the Raman spectrum of (ET)Au(C6Cl5)(4) confirms that the ET molecule in this salt is in the fl oxidation state. The variable temperature spin susceptibility data obtained from ESR spectroscopy indicate a weak ferromagnetic coupling between the radical ET+ cations. This salt provides the unique opportunity to investigate the properties of a highly isolated ET+ cation in the solid state.