HYDROTHERMAL SYNTHESIS AND STRUCTURAL CHARACTERIZATION OF A SERIES OFONE-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 be en prepared by hydrothermal methods and structurally characterized. Th e 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 diges tion 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 c onsists of one-dimensional chains of corner-sharing distorted {MoO4N2} octahedra. [Mo2O6(2,2'-bipy)] (2) was prepared from a mixture of Na2M oO4.2H(2)O, MoO3, 2,2'-bipyridine, MnCl2.4H(2)O, and H2O in the mole r atio 1:1:2:1.9:263 and was isolated as colorless plates. In contrast t o the structure of 1, compound 2 consists of a chain of alternating co rner-sharing {MoO4N2} octahedra and {MoO4} tetrahedra. Compound 3 was isolated as colorless octahedra. The structure of 3 consists of a chai n of corner-sharing {MoO4N2} octahedra and {MoO4} tetrahedra that alte rnate such that each {MoO4N2} octahedron corner-shares with another su ch octahedron and a {MoO4} tetrahedron; consequently, each {MoO4} unit corner shares with two {MoO4N2} octahedra. Crystal data: 1: monoclini c Cc, a = 14.246(3), b = 9.628(2), c = 7.344(1) Angstrom, beta = 101.2 6(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 = 10 4.888(1)degrees, V = 2367.76(7) Angstrom(3), Z = 4, D-calc = 2.088 g c m(-3), structure solution and refinement based on 5581 reflections con verged at R = 0.054.