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A series of 25 new organoantimony(V) cyanoximates has been synthesized and studied using IR, visible, and NMR spectroscopy and X-ray analysis. Crystal structures were determined for compounds (C₆H₅)₄Sb{ONC(CN)C(O)NH₂} (1) and (C₆H₅)₄Sb{ONC(CN)C(O)N(CH₃)₂} (2). Both complexes crystallized in the monoclinic space group P2₁/c (Z = 4) with unit cell parameters (Å, grad) of a = 14.921(3), b = 10.165(2), c = 17.571(7), β = 113.26(6) for compound 1, and a = 16.415(4), b = 10.406(3), c = 17.152(3), β = 117.79(2) for compound 2. For 5438 and 5056 independent reflections the refinement yielded R-factors 0.022 and 0.037 for the structures of 1 and 2, respectively. Cyanoxime anions are bound to the antimony(V) atoms in a monodentate fashion via the oxygen atoms of the oxime groups. The ligands adopt trans-anti configuration in these compounds. The coordination polyhedron in both complexes is a …