Inorganic Chemistry, Vol.43, No.6, 1964-1968, 2004
A novel organic-inorganic hybrid based on an 8-electron-reduced keggin polymolybdate capped by tetrahedral, trigonal bipyramidal, and octahedral zinc: Synthesis and crystal structure of (CH3NH3)(H(2)bipy)[Zn-4(bipy)(3)(H2O)(2)(MO8MoVI)-Mo-V O-4(36)(Po-4)]center dot 4H(2)O
Hydrothermal reaction of H3PO3, CH3NH2, zinc(II) acetate, 4,4'-bipyridine (bipy), and (NH4)(6)Mo7O24.4H(2)O at 180 degreesC led to a novel organic-inorganic layered hybrid, [CH3NH3][H(2)bipy][Zn-4(biPY)(3)(H2O)(2)(Mo8MoO36)-Mo-v-O-V1(PO4)] .4H(2)O (1). Its structure was established by single-crystal X-ray diffraction. It crystallizes in the monoclinic space group P2(1)/c with cell parameters of a = 17.3032(2), b = 17.8113(3), and c = 23.4597 (4) Angstrom, beta = 106.410(l)degrees, V = 6935.6(2) Angstrom(3), and Z = 4. The structure of compound 1 features a novel 2D layer built from the 8e-reduced tetracapped Keggin [Zn4Mo12O36(PO4)](3-) anions, which are further interconnected by bridging bipy ligands. The four zinc(II) ions are in tetrahedral, trigonal bipyramidal, and octahedral coordination geometries, respectively.