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The EPR spectrum of VO 2+  has been studied in single crystals of K 2 Zn(SeO 4 ) 2  · 6H 2 O and Rb 2 Zn(SeO 4 ) 2  ∼ 6H 2 O at ∼9.45 GHz. VO 2+  substitutes for Zn 2+  have preferential orientations in the lattice. The V = O of the intense vanadyl center is nearly along the longest ZnH 2 O direction. Spin‐Hamiltonian parameters have been evaluated from single crystal as well as from powder spectra.