Solid-State Coordination Chemistry of Metal Oxides:  Hydrothermal Synthesis and Structural Characterization of o-Phenanthroline-Ligated Copper− and Zinc−Molybdenum Oxides

The hydrothermal chemistry of molybdate with phenanthroline in the presence of M(II) cations was investigated. With Cu(II) starting materials, modifications in reaction conditions yielded the molecular cluster [Cu(o-phen)(2)Mo(4)O(13)] (MOXI-27) and one-dimensional [Cu(o-phen)MoO(4)].H(2)O (MOXI-28). The analogous Zn(II)-containing one-dimensional material [Zn(o-phen)MoO(4)] (MOXI-29) was isolated under conditions similar to those employed for the preparation of MOXI-28. Crystal data: C(24)H(16)CuMo(4)N(4)O(13) (MOXI-27), monoclinic, P2(1)/c, a = 10.5218(3) Å, b = 12.1113(4) Å, c = 22.0125(7) Å, beta = 97.988(1) degrees, Z = 4; C(12)H(10)CuMoN(2)O(5) (MOXI-28), monoclinic, P2(1)/n, a = 14.050(1) Å, b = 5.8818(4) Å, c = 16.227(1) Å, beta = 103.586(1) degrees, Z = 4; C(12)H(8)MoN(2)O(4)Zn (MOXI-29), monoclinic, P2(1)/m, a = 8.7714(7) Å, b = 6.4172(2) Å, c = 10.652(1) Å, beta = 100.702(5) degrees, Z = 2.