A time-resolved resonance Raman investigation of the reaction of the 2-fluorenylnitrenium ion with 2-fluorenylazide in a mixed aqueous solvent is presented. The reaction of the 2-fluorenylnitrenium ion with 2-fluorenylazide in the mixed aqueous solution generates two new species on the microsecond time scale. One of these species is identified as 2,2'-azobisfluorene, and the other species is tentatively assigned to a 1,4-bis-(2,2'-fluorenyl)-tetrazadiene cation intermediate. The structure and properties of these two species are briefly discussed. The reaction of the 2-fluorenylnitrenium ion with 2-fluorenylazide is also briefly compared to that of the 2-fluorenylnitrenium ion reactions with guanosine and water.