Nanostructured, mesoporous inorganic–organic hybrid xerogels were reproducibly synthesized by a sol–gel procedure. For the introduction of long alkyl chains into inorganic polymers, trifunctional n‐alkyltrialkoxysilanes of the type CH3(CH2)nSi(OR)3 (n = 7, 11, 17; R = CH3, C2H5) were co‐condensed with Si(OEt)4 (TEOS). The synthetic pathway involves the employment of n‐hexadecylamine as template and catalyst. The xerogels obtained by the present procedure consist of uniform spherical particles with a diameter of about 1 μm. The composition of the new materials was determined by 13C and 29Si cross polarization magic angle spinning (CP/MAS) NMR spectroscopy. In addition, the degree of organization was investigated by small angle X‐ray and electron diffraction. In accordance with 13C CP/MAS NMR spectroscopic measurements, the alkyl chains form a crystalline arrangement within the silica polymer. Brunauer–Emmett–Teller (BET) adsorption measurements confirm specific surface areas of up to 1400 m2/g. The material properties prove the xerogels to be suitable as stationary phases in high‐performance liquid chromatography (HPLC). These novel mesoporous, nanostructured materials have been successfully employed in HPLC for the first time. Different standard reference materials (SRMs) containing polycyclic aromatic hydrocarbons have been separated with the xerogels described in the present work.

Keywords: Iridium / Immobilization / Sol-gel processes / Accessibility studies / NMR spectroscopyThe synthesis of the T-silyl functionalized, and therefore solgel processable, Vaska complex [IrCl(CO){(C 6 H 5 ) 2 PC 6 H 4 -(CH 2 ) 4 Si(OMe) 3 } 2 ] [4(T 0 )] succeeded by reaction of [Ir(µ-Cl)(COE) 2 ] 2 (COE = cyclooctene; 1) with the phosphane (C 6 H 5 ) 2 PC 6 H 4 (CH 2 ) 4 Si(OMe) 3 [3(T 0 )] in the presence of carbon monoxide. Subsequently, 4(T 0 ) was co-polycondensed with five equivalents of (MeO) 3 Si(CH 2 ) 3 C 6 H 4 (CH 2 ) 3 Si(OMe) 3 {5[Ph(1,4-C 3 T 0 ) 2 ]} to give the polysiloxane-bound complex X1. For accessibility studies of the reactive centers, X1 was

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