Members of a new class of complexes, 2(CF3), 2(H), 2(Br), 2(I), and 2(OCH3), have been synthesized by a one-pot method involving the treatment of osmanaphthalynes bearing corresponding substituents (1(CF3), 1(H), 1(Br), 1(I), and 1(OCH3) with trimethylphosphine (PMe3) and water (H2O).