The structures of single crystals of [bipyH]+ [Fen,(ox)2(H20)2]-iH20 (1) and of a photoreaction product of 1, namely of single crystals of a 3-dimensional polymeric compound [FeII(bipy)3]2+"[FeII2(ox)3]"* 12"-(2), where ox is oxalate and bipy is 2,2'-bipyridine, have been determined by X-ray diffraction. Crystal data: 1, monoclinic, /lei, a = 7.302(2) A, b = 23.046(3) A, c = 10.361(2) A, ß = 91.12(2)°, Z = 4, R(F0) = 0.040 for 3273 independent data [/ > 3 (/); 2, cubic, P4332, a = 15.392(2) A, Z = 4, R(F0) = 0.050 for 1594 independent data [/ > 3 (/)].[Fen(ox)3/2]-units in 2 build a 3-dimensional anionic network. It can be described as a 3-connected net consisting of 10-gons, wherein the [Fe(bipy)3]2+ cations occupy the vacancies in an elaborate manner. There exist very few examples as yet of inorganic compounds with structures based on 3-dimensional 3-connected nets.
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