Abstract
Single crystals of the new quaternary compound In4Ti1.5Mo0.5Mo14O26 were obtained by solid state reaction. The crystal structure was determined by single-crystal X-ray diffraction. In4Ti1.5Mo0.5Mo14O26 crystallizes in the orthorhombic space group Pbca with unit-cell parameters a=9.4432(14)Å, b=11.4828(12)Å, c=20.299(4)Å and Z=4. Full-matrix least-squares refinement on F2 using 3807 independent reflections for 219 refinable parameters resulted in R1=0.0259 and wR2=0.0591. The crystal structure contains in addition to Mo14 clusters the first examples of mono- and bi-capped trioctahedral Mo14 i.e. Mo15 and Mo16 clusters. The oxygen framework derives from a stacking along the a direction of close-packed layers with sequence (…ABAC…). The Mo–Mo distances range between 2.6938(5) and 2.8420(6)Å and the Mo–O distances between 1.879(5) and 2.250(3)Å, as usually observed in molybdenum oxide clusters. The indium atoms form In46+ bent chains with In–In distances of 2.6682(5) and 2.6622(8)Å and the Ti atoms are in highly distorted octahedral sites of oxygen atoms with Ti–O distances ranging between 1.865(4) and 2.161(4)Å. Magnetic susceptibility measurements confirm the presence of Ti4+ cations and the absence of localized moments on the Mo network. Electrical resistivity measurements on a single crystal of In4Ti1.5Mo0.5Mo14O26 show a semimetallic behavior.
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