Flux synthesis of three-dimensional open-framework zinc phosphite and manganese phosphite-oxalate with 12-ring channels

Abstract

New three-dimensional open-framework zinc phosphite and manganese phosphite-oxalate, H 2dah·Zn 3(HPO 3) 4 ( 1) and H 2dab·Mn 2(HPO 3) 2(C 2O 4)(H 2O) 2 ( 2), were prepared in a flux of phosphorous acid without the addition of water as a solvent (dah = 1,7-diaminoheptane, dab = 1,4-diaminobutane). Compound 1 is constructed from strictly alternating ZnO 4 tetrahedra and HPO 3 pseudo pyramids, and has zigzag 12-ring channels running along the [0 0 1] direction. Compound 2 consists of neutral manganese phosphites layers, which are pillared by oxalate ligands to form a three-dimensional hybrid framework with 12-ring channels running along the [0 1 0] direction. Magnetic susceptibility measurements demonstrate the existence of antiferromagnetic interaction in 2. Crystal data: 1, orthorhombic, Pbcn, a = 9.9096(8) Å, b = 15.6780(6) Å, c = 13.8022(6) Å, V = 2144.3(2) Å 3, Z = 4; 2, monoclinic, P2 1/ n, a = 5.616(3) Å, b = 15.431(3) Å, c = 9.445(3) Å, β = 91.72(2)°, V = 818.2(5) Å 3, Z = 2.