[99Tc(phen)3]Cl2 was synthesized by reduction of pertechnetate with sodium borohydride in the presence of an excess of 1,10-phenanthroline and characterized by FAB mass spectrometry, magnetic susceptibility measurements, and i.r./vis/u.v. spectrophotometry. For biodistribution evaluation in mice [99mTc(phen)3]Cl2 could be obtained in a radiochemical purity of 92.5% using a similar procedure. The rather hydrophilic chelate was predominantly excreted by the kidneys. Its low blood retention resulted in a heart/blood activity ratio of 4.2 at 100 min post-injection.