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The previously reported preparations of [Mo bipy3]Cl3 and [Mo phen3]Cl3 have been reinvestigated and found to result in mixtures of (bipyH)[MoCl4 bipy], [Mo2O3Cl4 bipy2], NH4[MoCl4 bipy] and (phenH)[MoCl4 phen], [Mo2O4Cl2 phen2],H2O, K(phenH)2[MoCl6], respectively. All attempts to prepare [Mo bipy3]Cl3 and [Mo phen3]Cl3 have been unsuccessful. [MoCl2 bipy2][MoCl4 bipy] has been prepared from the direct reaction of K3MoCl6 and bipyridine under vacuum. [MoCl3 py phen] and [MoCl3 py bipy] have been obtained from [MoCl3 py3]. Infrared and visible spectra of the compounds are discussed along with the e.s.r. spectrum of [MoOCl3 bipy].