. Can. J. Chem. 69, 397 (1991). The reaction of NH4Tc04 with PPh3 in DMF solution in the presence of HCI produces mer-~c~~'(~~h~)~cl,(~MF).2PPh~ (1). When the reaction is done in acidic DMA, the yellow product isolated was identified as NH2(CH3)2+DMAH+ [ T c C~~]~-. P P~~O (2). The dimethylammonium cation was produced from the reaction of the solvent (DMA) with aqueous HCl. The reaction of NH4Tc04 with PPh3 in acidic acetone solution produces yellow (PPh3H)2[TcC16] (= 15% yield) and some orange crystals (=65% yield) identified by X-ray diffraction as