A dehydrocoupling polycondensation method for synthesizing polymetalloles including obtaining a dihydrometallole that includes silicon or germanium atoms, designating a reducing agent for preparation of dihydrometallole monomer, measuring a predetermined molar percentage of the reducing agent corresponding to a molar amount of the dihydrometallole, selecting a catalyst, and reacting the catalyst with the dihydrometallole to obtain a polymetallole. A method for detecting an analyte that may be present in ambient air or complex aqueous media including providing a polymer or copolymer containing a metalloid-metalloid backbone, exposing the polymer or copolymer to a suspected analyte or a system suspected of including the analyte, and measuring a quenching of photoluminescence of the metallole polymer or copolymer exposed to the system.