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Orthorhombic Mo-V oxide is one of the most active solid-state catalysts for selective oxidation of alkane, and revealing its detailed structure is important for understanding reaction mechanisms and for the design of better catalysts. We report the single-crystal X-ray structure analysis of orthorhombic Mo-V oxide heated under a N 2 flow; V is present in 6-membered rings with partial occupancy, similar to the structure reported by Trunschke's group for orthorhombic Mo-V oxide heated under an Ar flow (Trunschke, ACS Catal.2017, 7, 3061). Our previous paper (Ishikawa, J. Phys. Chem. C, 2015, 119, 7195) reported that V is not present in the 6-membered rings when orthorhombic Mo-V oxide is calcined in the presence of oxygen. Furthermore, Trunschke's paper reported that V in the 6-membered rings moves to the surface of the crystals under oxidation reaction conditions in the presence of H 2 O. Our present results provide additional evidence for V migration in the 6-membered rings during heat treatment. We also report the differences in the thermal behaviors, ultraviolet-visible absorptions, N 2 isotherms, and elemental analysis results of Mo-V oxide heated in air and under a N 2 flow. Furthermore, we report the solid-state transformation of orthorhombic Mo-V oxide to tetragonal Mo-V oxide by controlled heat treatment.

Thermal Behavior, Crystal Structure, and Solid-State Transformation of Orthorhombic Mo–V Oxide under Nitrogen Flow or in Air