This work presents the first full series of mixed precious-group metal-organic frameworks (MPG-MOFs) using ruthenium and rhodium. The obtained crystalline, highly porous and thermally robust materials were characterized by means of powder X-ray diffraction, N/CO sorption isotherms, thermogravimetry, spectroscopy methods (IR, Raman, UV/VIS-, NMR and XPS) and as well by high resolution transmission electron microscopy (HR-TEM) with elemental mapping (HAADF-EDS). Additionally, the assignment of spectroscopic data is supported by computational (time dependent)-density functional theory methods. The materials turned out to consist of homogeneously dispersed Ru and Rh paddlewheel units being linked by benzenetricarboxylate (BTC) to yield a framework that is isoreticular to [Cu(BTC)] (HKUST-1, Hong Kong University of Science and Technology). However, acetate (OAc) is incorporated as an intrinsic component which compensates for missing BTC-linker defects and some Cl is coordinated to the Ru centre at an apical position. The exact empirical formula of the MPG-MOFs is derived as [RuRh(BTC)(OAc)(Cl)].
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