The interaction of rhenium(III) halides ReBr and ReI with aqueous solution of sodium cyanide resulted in the formation of the first trinuclear halide-cyanide rhenium cluster complexes [{ReX}(CN)]/[{ReX}(CN)] (X = Br or I) crystallized as salts of the compositions CsNa[{ReBr}(CN)]·5.25HO (), CsNa[{ReI}(CN)]·6HO (), Cs[{ReBr}(CN)]·2HO·0.5CsCl (), and Cs[{ReI}(CN)]·(). All of the compounds are stable in air in the solid state and in aqueous solution. The substitution of apical halide ligands in the parent compounds ReX by cyanides led to reduction of the original metallocluster Re (12 cluster valence electrons (CVEs)) to Re (14 CVEs), forming the compounds and . The apical CN ligands affect the electronic structure of the Re metallocluster stabilizing reduced form. Complexes and represent the first examples of triangular rhenium clusters with the Re metallocluster. The reaction of and with HO resulted in formation of compounds and with the formal charge of the Re metallocluster equal to 8+, and no further oxidation to Re occurred. The compounds were characterized by the X-ray diffraction analysis, NMR and UV-vis spectroscopies, mass spectrometry, cyclic voltammetry, and magnetic susceptibility measurements.
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