The proton magnetic resonance spectra of a number of coba1t(111), molybdenum(0), chromium(0), platinum(11) and palladium(11) complexes of (R)-propane-1,2-diamine, (S)-3,3-dimethylbutane-1,2- diamine, (RS)-N,N,N',N?-tetramethylpropane-1,2-dime and ethane-1,2-diamine have been analysed and the coupling constant data utilized to calculate the conformational populations for the various complexes. Necessary parameters for the conformational analysis were obtained from a study of tetracyano{(S)-3,3-dimethylbutane-1,2-diamine)cobaltate(111),in which the t-butyl group was assumed to be exclusively in the equatorial orientation. The preparation and resolution of this t-butyl substituted ethane-1,2-diamine are described.