Preparation and Structure of Tetraphenylarsonium Bis(Benzene-1,2-Dithiolato)Oxotechnetate(V)

Abstract

The reaction of benzene-1,2-dithiol (bdtH₂) with [AsPh₄] [TcOCl₄] in aqueous alcohol yields crystals of [AsPh₄] [ TcO ( bdt )₂] (1) from acetonitrilelethanol. The crystal structure of (1) has been determined by X-ray diffraction and found to be isostructural with [PPh₄] [ MoO ( bdt )₂]. Crystals art monoclinic and belong to the space group Cc with a 12.652(1), b 15.783(1), c 16.622(1) Å, β 93.03(1)º with Z 4. Refinement on 2828 diffractometer data measured with Cu Ka radiation converged at R 0.030. The structure consists of [ TcO ( bdt )₂]- anions and [AsPh₄]⁺ cations. The technetium(V) atom is five-coordinate, with the four sulfur atoms in the basal positions and the oxo ligand in the apical position, to give a distorted square-pyramidal environment about the technetium.