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The article provides new data about characteristics of the organic matter and mineralogical composition of the Cape Muostakh sediments related to intense permafrost degradation (thermoerosion processes). The sedimentary material has been investigated by X-ray diffraction, GC-MS, IRM-GC-MS, pyrolysis–gas chromatography–mass spectrometry (Py–GC–MS), and Rock-Eval pyrolysis. Variable distribution of the total organic carbon content over the coast cliff is established. The minimum content of the organic carbon occurs at the cliff level of 5 m above sea level, and the maximum is located on the top of the cape cliff. The practical absence of unsaturated compounds indicates the intense destruction of the ice complex deposits that occurred at the level of 5 m of the Cape Muostakh cliff. The minimum organic carbon, aliphatic compounds, and the increase of the ?13C indicates the loss of hydrogen-enriched organic matter, while condensed carbon structures remain in sediment. Aromatic compounds of both plant and petroleum origin were identified in all sediments, except in the sediment sample collected at the cliff level of 5 m. Unsaturated fatty acids were detected only in the sediments of the upper cliff levels. The novel hopenes and hopane were detected and they predominantly occur in the upper layers of the cape cliff.