The 1:1 M reaction of MoCl5 with Cl(CH2)(2)OH, in dichloromethane at room temperature, proceeded with chlorine-oxygen interchange and HCl release to give MoOCl3 in 65% yield. The analogous reactions involving 'PrOH, MeOH, L-menthol and H2O gave impure MoOCl3. MoCl5 reacted with Me2N(CH2)(2)OH in 1:1 M ratio affording the 2-chloroammonium salt [Me2NH(CH2)(2)Cl](2)[Mo2O2Cl8], 1. The reaction of MoCl5 with MeO(CH2)(2)OH afforded a mixture of [Mo((KO)-O-2,O'-O(CH2)(2)OMe)(2)Cl-2][MO2O2C17], 2a, and [Mo(K-2,O,O'(CH2)(2)OMe)(2)Cl-12][MoOCl4], 2b. The products 1, 2a and 2b were characterized by analytical and spectroscopic techniques, and by X-ray diffractometry. The X-ray structure of 2b shows weak anion-anion interactions, therefore 2b might be ...