Graduation qualification work is associated with the development of fundamental concepts of the structure and methods of synthesis of an important class of complex inorganic compounds - perovskite-like layered phases, built on a block principle by alternating blocks of perovskite structure and fragments of other structural types. This work was carried out in cooperation with the Faculty of Chemistry of St. Petersburg State University within the framework of the RFFI project "Topochemical processes in protonated and intercalated layered perovskite-like materials: thermochemical and structural studies". Specifically, in order to study in this paper, a study was made of the structure of protonated perovskite-like layered structures described by the general formula A2R2Ti3O10 (A = H, Rb, H / Rb, R = La, Nd), considered as promising for use as photocatalysts because of the possibility Intercalation of water into interlayer space. The result of this phenomenon is an increase in the working surface of the photocatalyst, what leads to an increase in its efficiency. To record the possibilities for intercalation, X-ray diffraction was used, because this process is directly related to the increase in lattice parameters. Further M.R. Gilmiyarov expanded the class of information that can be extracted from the diffraction data and deciphered the crystal structures of the samples: spatial groups, atomic positions in the unit cell and the population of positions; carried out an analysis of structural changes at various protonation rates. M.R. Guilmiyarov independently carried out a complete analysis of all the obtained X-ray and synchrotron diffraction experimental data. For the skilled execution of all calculations, he needed to master the method of full-profile analysis of powder diffraction patterns and his software implementation in the package FullProf_Suite. First, a preliminary determination of lattice parameters and a spatial group was made on the basis of the DICVOL program. After that, the crystal structure was refined by the methods of Le Bail and Rietveld. The first results of the presented work on the indications of the X-ray diffraction patterns of the studied compounds have already been reported at two youth conferences: International Student Conference "Science and Progress" October 17-21, 2016 St. Petersburg - Peterhof and the Youth Science Forum "Open Science 2016" November 16-18, 2016 in Gatchina. I think that the graduate qualification work of the student Gilmiyarov Marat Rafaelevich deserves an assessment "excellent", and he deserves awarding a bachelor's degree in the direction of 03.04.02 "Physics". I also consider it necessary to continue the research that has begun, so I recommend M.R. Gilmiyarov for admission to the master's program of St. Petersburg State University.