Hydrothermal synthesis and characterization of two novel three-dimensional vanadium phosphites: |(C10H10N2)|V2IVO2(HPO3)2(H2PO3)2 and |(C4H16N3)|V2IVVIIIO2F2(HPO3)4

Abstract Two novel three-dimensional vanadium phosphites |(C 10 H 10 N 2 )| V 2 IV O 2 ( HPO 3 ) 2 ( H 2 PO 3 ) 2 1 and |(C 4 H 16 N 3 )| V 2 IV V III O 2 F 2 ( HPO 3 ) 4 2 have been synthesized hydrothermally in the presence of structure-directing agents. Single-crystal structural analysis reveals that compound 1 has a three-dimensional open-framework with two different types of intersecting channels (monoclinic, P 2 1 / n , a  = 6.3541(14) A, b  = 10.460(2) A, c  = 14.769(3) A, β  = 90.412(5) o , V  = 981.6(4) A 3 , Z  = 2 with R 1  = 0.0523), while compound 2 (orthorhombic, Pbca , a  = 13.612(3) A, b  = 9.5753(19) A, c  = 14.022(3) A, V  = 1827.6(6) A 3 , Z  = 4 with R 1  = 0.0441) presents a three-dimensional open-framework that consists of a novel {V 3 O 14 F 2 } trimer with mixed valence V 2 IV V III linked by two bridging F atoms. In addition, it is worth noting that the organic templates play important roles in the formation of both novel structures. Further characterization of the two compounds has been performed, including X-ray powder diffraction, ICP, CHN, IR and TG–DTA analyses.