The new mononitrosyl complexes [Mo(NO)LI(OC 6H 4CO 2C 12H 25)], [Mo(NO)LC1(OC 6H 4CO 2C 12H 25)], [Mo(NO)L(OC 6H 4CO 2C 12H 25) 2], [Mo(NO)LI(NHC 6H 4C 10H 21)], [Mo(NO)LC1(NHC 6H 4C 10H 21)] and [Mo(NO)L(NHC 6H 4C 10H 21) 2] [L = HB(3,5-Me 2C 3N 2H) 3] have been synthesized and characterized by spectroscopic methods. All undergo one-electron reduction processes at potentials ranging from −0.18 to −1.40 V (SCE). These new compounds have been examined by differential scanning calorimetry. Although these compounds have reduced melting points compared to compounds lacking long alkyl chain substituents, 44°C in the case of the bis-phenoxide derivative, none exhibits liquid crystalline behaviour.