Nitric oxide (NO) is one of the main environmental pollutants and one of the biomarkers noninvasive diagnosis of respiratory diseases. Organic-inorganic hybrids based on heterocyclic Ru (II) complex and nanocrystalline semiconductor oxides SnO 2 and In 2 O 3 were studied as sensitive materials for NO detection at room temperature under periodic blue light (λ max = 470 nm) illumination. The semiconductor matrixes were obtained by chemical precipitation with subsequent thermal annealing and characterized by XRD, Raman spectroscopy, and single-point BET methods. The heterocyclic Ru (II) complex was synthesized for the first time and characterized by 1 H NMR, 13 C NMR, MALDI-TOF mass spectrometry and elemental analysis. The HOMO and LUMO energies of the Ru (II) complex are calculated from cyclic voltammetry data. The thermal stability of hybrids was investigated by thermogravimetric analysis (TGA)-MS analysis. The optical properties of Ru (II) complex, nanocrystalline oxides and hybrids were studied by UV-Vis spectroscopy in transmission and diffuse reflectance modes. DRIFT spectroscopy was performed to investigate the interaction between NO and the surface of the synthesized materials. Sensor measurements demonstrate that hybrid materials are able to detect NO at room temperature in the concentration range of 0.25-4.0 ppm with the detection limit of 69-88 ppb.Nanomaterials 2020, 10, 70 2 of 22 in noninvasive diagnosis of respiratory diseases [7][8][9]. In this case, the limitation of the quantitative determination of NO in exhaled air is due to the low level of its concentration (20-200 ppb) among a wide range of interfering gases [10].Direct determination of nitrogen monoxide in the gas phase is possible using conductometric gas sensors based on various semiconductor metal oxides [7,[10][11][12][13][14][15][16][17][18][19][20][21][22]. To increase selectivity of such analysis along with lower power consumption, complete or partial replacement of thermal heating with photoactivation is a promising approach. Activation of the sensor response under illumination occurs through various mechanisms depending on the nature of the target gas. For oxidizing gases (NO 2 , O 3 ), which compete with oxygen for the same adsorption sites, photogeneration of electron-hole pairs plays a major role in the photodesorption process. On the contrary, for the detection of reducing gases (CO, NH 3 , H 2 S), the presence of chemisorbed oxygen on the surface of the semiconductor oxide is necessary. In this case, the increase in the sensor response under illumination is due to the unpinning of Fermi level of the semiconductor. In most works NO is detected as oxidizing gas. The similar routes of NO and NO 2 sensing was recently evidenced by in situ DRIFT spectroscopy [23]. Our previous works show that highly selective NO 2 detection is possible using visible light photoactivation [24][25][26][27]. To shift the optical sensitivity of semiconductor oxides into the visible range, it is necessary to create defects in the semiconductor matrix or i...