Single crystals of MnUO 4 , FeUO 4 , and NiU 2 O 6 were grown for the first time. The use of chloride fluxes facilitated the crystal growth. MnUO 4 , a hexavalent uranium compound, crystallizes in the orthorhombic space group, Imma, with a = 6.6421(19) Å, b = 6.978 (2) Å, and c = 6.748 (2) Å, and exhibits typical uranyl, UO 2 2+ , coordination. FeUO 4 and NiU 2 O 6 contain pentavalent uranium and are structurally related, exhibiting threedimensional connectivity. FeUO 4 crystallizes in the orthorhombic space group, Pbcn, with a = 4.8844(2) Å, b = 11.9328(5) Å, c = 5.1070(2) Å. NiU 2 O 6 crystallizes in the trigonal space group, P321, with a = 9.0148(3) Å, c = 5.0144(3) Å.