Oxygen-sensitive and near-infrared( NIR) luminescent Yb III coordination polymers incorporatingl igandsb ased on pyrene derivatives were synthesized:Y b III -TBAPy and Yb III -TIAPy (TBAPy:1 ,3,6,8-tetrakis(p-benzoate)pyrene;T IAPy: 1,3,6,8-tetrakis(3,5-isophthalic acid)pyrene). The coordination structures of thesem aterials have been characterized by means of electrospray ionization mass spectrometry,X -ray diffractiona nalysis, and thermogravimetric analysis. Moreover,t he porouss tructure of Yb III -TIAPy has been evaluated by measuring its N 2 adsorption isotherm.T he NIR lumines-cence properties of Yb III -TBAPy and Yb III -TIAPy have been examined by acquiring emission spectra and determining emission lifetimes under air or argon and in vacuo. Yb III -TIAPy exhibitedh igh thermals tability (with ad ecomposition temperature of 400 8C), intensel uminescence (with an emission quantum yield under argon of 6.6 %), and effective oxygen-sensing characteristics. These results suggest that NIR luminescent Yb III coordination polymers prepared using pyrene derivatives could have applications in novel thermostable oxygen sensors.