The prime objective of the present work is evaluating the performance of double Perovskite material with Calcium in the A-site cation and Manganese and Cobalt in the B-site cation. The Ca2MnCoO6 the double Perovskite which is a compound of Calcium, Manganese with cobalt is made in the form of polycrystalline using the attached quartz pipe system. The partial oxygen pressure inside the quartz tube expressed this as an important set parameter for the production of a structural phase model. This parameter was controlled using the ratio between ReO2 and ReO3 content and the filling parameter (ratio between weight and total quartz tab content). Molecular and chemical components were investigated by scanning with electron microscopy and diffraction microscopy. The structural parameters of the crystal were determined by analyzing the X-ray powder distribution pattern with high resolution synchrotron. The analysis indicates that the sample is a single-layer compound compatible with the monolin crystal structure. (Space group P21/n) with a = 5.3649 (2) Å; b = 5.49863 (3) Å; c = 7.77524(3) Å; and β = 90.19(1)º. Computer simulations were performed considering two cation valence settings, that is, (i) Mn2+Re6+ or (ii) Mn3+Re5+, for the Ca2MnCoO6 compound. XANES analysis measurements indicated +2.4 for the means valence of Mn (a mixture of Mn2+ and Mn3+) and +5.8 for the effective valence of Re (an intermediate valence between Re4+ (ReO2) and Re6+ (ReO3)). In summary, we concluded that Ca2MnCoO6 Mn and Re have a mixed valence configuration based on oxygen content of 6.0±0.2.