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[Display omitted] • Fluorinated graphite (FG) CF 0.4 is irradiated with a synchrotron white beam. • XPS spectra showed little change in the composition of the irradiated layers. • Under photon action, HNO 3 , NO 2 , NO, and N 2 decompose inside the FG matrix. • Embedded NO x molecules stimulate FG defluorination and vacancy formation. • Nitrogen from NO x molecules saturates the boundaries of vacancies. Layered fluorinated graphite material can become an efficient nanoreactor for photochemical reactions. In this work, we compared the photochemical behavior of partially fluorinated graphite (FG) and FG containing nitrogen oxides in the interlayer space (NO x @FG) under the action of a high-intense polychromatic photon beam from the synchrotron radiation source BESSY II. Analysis of the chemical and electronic states of the samples was performed using X-ray photoelectron spectroscopy and near-edge X-ray absorption fine structure spectroscopy. Density functional theory calculations were used to interpret and analyze the experimental data. It was found that nitrogen oxides promote the photo-induced degradation of the FG matrix, namely, its partial defluorination, formation of vacancies and doping with nitrogen, while the empty FG had a high photoresistance to synchrotron radiation. The results obtained can be used in the development of new approaches to the modification of graphene layers and in the creation of photostable materials for optical elements. [ABSTRACT FROM AUTHOR]