Ionic liquid of choline chloride/malonic acid as a solvent in the synthesis of open-framework iron oxalatophosphates

Two new iron(III) oxalatophosphates, Cs2Fe(C2O4)(0.5)(HPO4)(2) (1) and CsFe(C2O4)(0.5)(H2PO4)(HPO4) (2), have been synthesized by using a low melting point eutectic mixture of choline chloride and malonic acid as a solvent and characterized by single-crystal X-ray diffraction and magnetic susceptibility. Crystal data are as follows: compound 1, monoclinic, P2(1)/c (No. 14), a = 8.5085(4) angstrom, b = 12.7251(6) angstrom, c = 9.8961(4) angstrom, beta = 107,117(1)degrees, V = 1024.01(8) angstrom(3), Z = 4, and R-1 = 0.0264; compound 2, monoclinic, P2(1)/n (No. 14), a = 8.0038(3) angstrom, b = 10.2923(3) angstrom, c = 11.4755(4) angstrom, beta = 100.507(1)degrees, V = 929.47(5) angstrom(3), Z = 4, and R-1 = 0.0311. The structure of 1 comprises FeO6 octahedra connected by HPO42- tetrahedra and bisbidentate oxalate anions to form a 3D framework containing intersecting 12-ring channels, with the charge-compensating Cs+ cations being located at the intersections of these channels. The structure of 2 consists of 2D layers of octahedral FeO6, tetrahedral H2PO4- and HPO42- moieties, and bisbidentate oxalate ligands with the Cs+ cations between the layers. They are the first examples for the use of ionic liquid as a solvent in the synthesis of metal oxalatophosphates.