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The reaction of MoCl62" or MoCl6" with Mo(CO)4Cl3~inCH2Cl2 results in the formation of Mo2Cl,3" and MoCl92", respectively. The temperature dependence of the magnetic moment of the latter is shown to be hi accord with the thermal equilibrium 5 = */2 4* S = 3/2, while its infrared spectrum can be readily assigned assuming a bioctahedral, D3h structure. It is easily reduced to Mo2C193_. The reaction of Mo2Cl92' with Mo(CO)4Cl3" leads to Mo3C1123" whose trinuclear structure was verified from conductivity measurements. Both the electronic and the infrared spectra are in accord with a linear, trioctahedral, face-shared structure (unlike Re3Cl123"). Magnetic moments in solution are in qualitative agreement with the thermal equilibrium 5 = '/2 & S = 3/2.

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