Investigation into the hydrothermal assembly of molybdenum polyoxoanion solids in the presence of 4-aminobenzoic acid, guanidinium carbonate, and aminoacetic acid

The hydrothermal synthesis of three novel molybdenum polyoxoanion solids in the presence of 4-aminobenzoic acid, guanidinium carbonate, and aminoacetic acid and their crystal structures are reported. The layer structure of 1 can be envisioned as bundles of parallel spirals of tetrameric building units connected via shared corners. Pseudo-one-dimensional 4- and 6-ring channels are found in the interlamella region. The chain structure of 2 consists of corner- and edge-sharing MoO6. Large interstrand separation is created due to the inclusion of CN3H6+. The structure of 3 consists of three-dimensional mixed covalent-hydrogen bonded [(NH3CH2COO)(2)Mo8O26](4-) with large pseudo-one-dimensional channels. Crystal data: H8Mo4N2O13 (1), orthorhombic Pbca, a = 7.682(5) Angstrom, b = 15.389(2) Angstrom, c = 18.996(4) Angstrom, V = 2246(2) Angstrom(3), Z = 8, 1972 reflections, R-1 = 0.034 [I > 2 sigma(I)]. CH10Mo3N4O10 (2), monoclinic P2(1)/c, a = 7.6158(13) Angstrom, b = 16.5768(11) Angstrom, c = 9.1946(8) Angstrom, beta = 95.237(8)degrees, V = 1155.9(2) Angstrom(3), Z = 4, 2020 reflections, R-1 = 0.0281 [I > 2 sigma(I)]. C2H15Mo4N3O16 (3), monoclinic C2/c, a = 17.326(4) Angstrom, b = 10.744(2) Angstrom, c = 18.697(4) Angstrom, beta = 108.27(3)degrees, V = 3305.0(12) Angstrom(3), Z = 8, 2896 reflections, R-1 = 0.0250 [I > 2 sigma(I)].