Inorganic-Organic Hybrid Materials: Synthesis and Structure of a Reduced Ferrous Molybdophosphate, [(C12H8N2)3FeII]2[Fe11MOV12(H2PO4)6(PO4)2(OH)6O24], in the Presence of Fe(II)(1,10-Phenanthroline)3 Complex

A new composite solid of the formula [(C12H8N2)3FeII]2 [FeIIMoV12(H2PO4)6(PO4)2(OH)6O24] 1 has been synthesized from a reaction mixture of MoO3, Fe2(C2O4)3·6H2O, C2H2O4·2H2O, 1,10-phenanthroline monohydrate, H3PO4, and H2O under hydrothermal conditions. Crystal data: trigonal, space group R-3, a=16.874(6) ?, c=30.117(7) ?, V=7426(4) ?3, R1 =0.0190, wR2=0.0468, and S=1.137. The structure of 1 is built up from FeMo12(H2PO4)6(PO4)2(OH)6O4-24 cluster anions connected to each other via hydrogen bonds. The arrangement of clusters is such that each cluster is surrounded by six equivalent anions resulting in three-dimensional cavities. The charge balancing cation, [(C12H8N2)3Fe]2+ complex, resides in the cavities and interact with the clusters through hydrogen bonds. There is also strong PI–PI interactions exist among the phenyl rings.