The limited scheelite type Cd 1−3x □ x Gd 2x MoO 4 solid solution, where 0<x≤0.25 and □ are cationic vacancies have been successfully synthesized by high-temperature annealing of CdMoO 4 /Gd 2 (MoO 4 ) 3 mixtures composed of 50.00mol.% and less of Gd 2 (MoO 4 ) 3 . The obtained materials as well as CdMoO 4 and Gd 2 (MoO 4 ) 3 were characterized by powder XRD, DTA–TG, DSC, and SEM techniques. A phase diagram of the pseudobinary CdMoO 4 –Gd 2 (MoO 4 ) 3 system was constructed. The eutectic point corresponds to 1350±5K and ∼70.00mol.% of Gd 2 (MoO 4 ) 3 in an initial CdMoO 4 /Gd 2 (MoO 4 ) 3 mixture. With decreasing of Gd 3+ amount in the crystal lattice of CdMoO 4 , a melting point of the Cd 1−3x □ x Gd 2x MoO 4 solid solution increases from 1351 (x=0.25) to 1408K (x=0). EPR method was used to identify the paramagnetic Gd 3+ centers in Cd 1−3x □ x Gd 2x MoO 4 for different values of x parameter as well as to select biphasic samples containing both Cd 0.2500 □ 0.2500 Gd 0.5000 MoO 4 and Gd 2 (MoO 4 ) 3 .