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BYA mechanistic and kinetic study has been made of the cisltrans-isomerisation of cis-azodioxycyclohexane and cis-azodioxymethane in acetonitrile at temperatures, varying from 0-60". Cross-over and trapping experiments show that the isomerisation does not proceed by rotation around the N-N bond but exclusively via dissociation and recombination of free monomer molecules. Kinetic data indicate that the monomer molecules dimerize at low temperature by kinetic control chiefly to the cb-isomer. At elevated temperatures the thermodynamically more stable trans-isomer is formed. Activation parameters show that the formation of the cis-isomer from two monomer molecules is controlled by entropy rather than by enthalpy factors.