The crystal and local structures of Czochralski-grown calcium orthovanadate (Ca(VO)) single crystals doped with over-stoichiometric 0.05 wt % MnO (CVO:0.05Mn) and annealed under different conditions are studied by single-crystal conventional and synchrotron X-ray diffraction, X-ray absorption spectroscopy, and electron paramagnetic resonance for the first time. Bottom (annealing in air) and top (annealing in air and in vacuum) parts of the CVO:0.05Mn crystal differ in the manganese content (higher in the bottom part), formal charge (Mn and Mn, respectively), and color (orange bottom part; light orange and yellow top parts annealed in air and vacuum, respectively). Manganese ions are located in one (Ca3, distorted two-capped trigonal prism) of five crystallographic Ca sites and have octahedral coordination, which is consistent with crystal-chemical properties of transition-metal ions. The presence of vacancies in one of three V sites is revealed. Formal charge 5+ for vanadium ions is confirmed by X-ray photoelectron spectroscopy. Different colors of CVO:Mn crystals and different formal charges of manganese are explained depending on the growth and post-growth treatment conditions.
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