Hydrothermal synthesis and structural characterization of a series of one-dimensional organic/inorganic hybrid materials of the [(MoO3)(n)(2,2'-bipy)(m)] family: [MoO3(2,2'-bipy)], [Mo2O6(2,2'-bipy)], and [Mo3O9(2,2'-bipy)(2)]

Three one-dimensional molybdenum oxide/2,2'-bipyridine species have been prepared by hydrothermal methods and structurally characterized. The reaction of MoO3, 2,2'-bipyridine, and H2O in the mole ratio 1:0.68:680 at 160 degrees C for 120 h in a 23 mt Teflon-lined Parr acid digestion bomb produces colorless rods of [MoO3(2,2'-bipy)] (1) mixed with colorless octahedra of [Mo3O9(2,2'-bipy)(2)] (3). The structure of 1 consists of one-dimensional chains of corner-sharing distorted {MoO4N2} octahedra. [Mo2O6(2,2'-bipy)] (2) was prepared from a mixture of Na2MoO4.2H(2)O, MoO3, 2,2'-bipyridine, MnCl2.4H(2)O, and H2O in the mole ratio 1:1:2:1.9:263 and was isolated as colorless plates. In contrast to the structure of 1, compound 2 consists of a chain of alternating corner-sharing {MoO4N2} octahedra and {MoO4} tetrahedra. Compound 3 was isolated as colorless octahedra. The structure of 3 consists of a chain of corner-sharing {MoO4N2} octahedra and {MoO4} tetrahedra that alternate such that each {MoO4N2} octahedron corner-shares with another such octahedron and a {MoO4} tetrahedron; consequently, each {MoO4} unit corner shares with two {MoO4N2} octahedra. Crystal data: 1: monoclinic Cc, a = 14.246(3), b = 9.628(2), c = 7.344(1) Angstrom, beta = 101.26(3)degrees, V = 987.9(3) Angstrom(3), Z = 4, D-calc = 2.018 g cm(-3); structure solution and refinement based on 1346 reflections converged at R = 0.026; 2: monoclinic P2(1)/m, a = 9.0875(6), b = 6.8286(5), c = 10.5441(7) Angstrom, beta = 99.307(2)degrees, V = 645.70(8) Angstrom(3), Z = 2, D-calc = 2.284 g cm(-3), structure solution and refinement based on 1607 reflections converged at R = 0.062; 3: monoclinic P2(1)/n, a = 13.5468(3), b = 10.1407(2), c = 17.8346(1) Angstrom, beta = 104.888(1)degrees, V = 2367.76(7) Angstrom(3), Z = 4, D-calc = 2.088 g cm(-3), structure solution and refinement based on 5581 reflections converged at R = 0.054.