Extended X-ray Absorption Fine Structure (EXAFS)was used to determine the molecular species obtained in the synergistic extraction of zinc by a benzene solution of TTA [thenoytrifluoro-acetone, or 4,4,4-(trifluoro-l-(2-thienyl)-l,3-butadione]and TBP (tributyl phosphate). The zinc in the extracted complex is surrounded by five oxygen atoms at a distance of 2.01 A. The coordination number is established by the zinc-oxygen distance, which is shown to be characteristic of this type of pentacoordinated zinc compound. The coordination number is also independently determined by direct comparison of an EXAFS function with those obtained from compounds of known structure. The coordination number is in agreement with that concluded by Nash and Choppin from thermodynamic results. The Debye-Waller term for a series of zinc crystals and solutions is discussed.