A new polymorph of CeNiSb3 has been grown from a Sn flux and characterized by single-crystal X-ray diffraction. beta-CeNiSb3 crystallizes in the orthorhombic space group Pbcm (No. 57) with Z = 8. The unit cell parameters are a = 12.9170(2) A, b = 6.1210(5) A, c = 12.0930(6) A, and V = 956.13(9) A3. Its layered structure contains structural motifs similar to that of the first form of CeNiSb3 and consists of Ce atoms inserted between anionic layers of nearly square infinity2[Sb] nets and distorted infinity2[NiSb2] octahedra. We report the synthesis, magnetization, electrical resistivity, and specific heat of the new form of CeNiSb3 and compare the structures and physical properties of both polymorphs.