Single crystals of a Re(VII) complex, the dihydrogenophosphato phenanthroline trioxo-rhenium monohydrate of formula [ReO 3 (phen)(H 2 PO 4 )]·H 2 O (phen = 1,10-phenanthroline), were prepared in aqueous solution. X-Ray analysis shows that it crystallizes in the monoclinic space group P2 1 /c with the unit cell parameters: a = 8.611(2), b = 13.881(2), c = 14.502(4)Å, β = 120.87(2) • , V = 1487.9(6)Å 3 and Z = 4. In the neutral complex, the rhenium is in the oxidation state +VII, coordinated by two nitrogen atoms of the bidentate phen, three terminal oxygen atoms and, for the first time, one oxygen atom of the mono-deprotonated phosphoric acid ligand H 2 PO − 4 , forming a squarebased bipyramidal coordination geometry. The thermal stability, IR, UV/Vis and fluorescence spectroscopic properties are given. The complex shows antimicrobial activity against five different microbes.