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Nanostructured heterolayered compounds based on molybdenum disulfide are formed due to self-assembly of negatively charged single MoS2 layers and guest organic cations in liquid medium. Unique charge-transporting and catalytic properties of such systems stimulate the studies of their synthesis and relationship between the nature of organic guests and compounds structure. In the present communication, the structure of new layered nanocrystals, containing protonated forms of ethylenediamine, tetramethylethylenediamine and hexamethylenediamine in-between the МoS2 layers, is reported. Atomic structure of the host and guest layers was determined from powder X-ray diffraction data, using an original approach previously developed for related compounds [1,2]. According to the structure determination results obtained by the PXRD pattern modeling, DFT calculations, FTIR, and TEM study, the organic−inorganic hydrogen bonding interaction is an important structure-forming factor in the present nanoorganized heterolayered systems. The strong NH···S interactions contribute to their stabilization, being accompanied by the contribution of weaker but more numerous CH···S interactions. The latter impact depends on the nature and geometry of alkyl fragments in molecule and can be comparable in magnitude with that of strong hydrogen bonding. The geometry adapted by the MoS2 layers was found to be similar for all three studied NCs. It is modified by the charge transfer to the sheets of starting MoS2, resulting in their change to 1T structure type, promising for many important applications [3]. The funding of the work by the Russian Foundation for Basic Research (grant 16-29-06184-ofi-m) is gratefully acknowledged. References [1] Goloveshkin A.S., Lenenko N.D., Zaikovskii V.I., Golub A.S., Korlyukov A.A., Bushmarinov I.S. // RSC Adv, 2015, 5, 19206–19212. [2] Goloveshkin A.S., Bushmarinov I.S., Korlyukov A.A., Buzin M.I., Zaikovskii V.I., Lenenko N.D., Golub A.S. // Langmuir, 2015, 31, 8953–8960. [3] Ivan E. Ushakov, Alexander S. Goloveshkin, Natalia D. Lenenko, Mariam G. Ezernitskaya, Alexander A. Korlyukov, Vladimir I. Zaikovskii, and Alexandre S. Golub // Crystal Growth and Design, 2018, 18 5116-5123