Synthesis and structure of a bimetallic hybrid inorganic/organic layered coordination polymer with an octamolybdate cluster variant trapped between the α and δ isomeric forms |
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Institution: | Lyman Briggs College and Department of Chemistry, Michigan State University, MI 48825, USA |
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Abstract: | Hydrothermal combination of CuSO4, MoO3, and 4-phenylpyridine (4-phpyr) in a 1:4:4.5 ratio under basic conditions afforded purple crystals of {Cu(4-phpyr)4]2(Mo8O26)·4-phpyr} (1), which were analyzed by spectroscopy and single crystal X-ray diffraction. The asymmetric octamolybdate clusters in 1 adopt an intermediate structural variant between the known α and δ isomeric forms, with four octahedral and three tetrahedral molybdenum coordination spheres, along with one molybdenum atom in a highly distorted square pyramidal environment. Paddle-wheel shaped Cu(4-phpyr)4]2+ cations link adjacent {α/δ-Mo8O26}4− clusters into a 2-D layered rhomboid grid coordination polymer. Uncoordinated 4-phpyr molecules lie in incipient voids in the interlamellar regions. The structure of 1 illustrates the utility of sterically bulky coordination complexes in the stabilization of intermediate conformations during energetically facile polyoxometallate isomer interconversion. Crystallographic data: triclinic, P1, a = 13.717(3) Å, b = 13.728(3) Å, c = 14.809(3) Å, α = 109.251(4)°, β = 107.670(4)°, γ = 92.005(4)°, V = 2480.0(9) Å3, R1 = 0.0637, wR2 = 0.1054. |
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