PbMoxW1-xO4 single-crystal solid solutions with x=0.2, 0.5, 0.8 have been grown by the Czochralski method in air atmosphere from the initial charge with over-stoichiometric amount of YNb04 (15 wt%). X-ray and neutron single-crystal and X-ray powder (Rietveld method) diffraction investigations of PbMoxW1-xO4 crystals indicate bulk inhomogeneity of their compositions, absence of color centers, and deviation of refined compositions from initial ones: the Nb5+ and Y3+ contents as well as oxygen vacancies content increase with increasing x in PbMoxW1-xO4. It was found that PbMoxW1-xO4 with x=0.2, 0.5, 0.8, 1.0 crystallizes in the scheelite-type structure with space group I4(1)/a, unlike crystal with x=0, which is characterized by the symmetry reduction to space group I (4) over bar caused by ordering of oxygen vacancies. The correlation between the a and c unit cell parameters and composition of cation sites, dodecahedral and tetrahedral, and deficiency of oxygen site was revealed. (C) 2016 Elsevier Ltd. All rights reserved.