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Phosphorus-31 nmr data are reported for tri-n-butylphosphine selenide complexes of mercury(II) and cadmium halides and for some miscellaneous complexes of tertiary phosphine sulfides and selenides with the same metal halides. The ligands in the complexes are labile in solution at room temperature but the exchange can be "frozen out" in certain cases at reduced temperature. Selenium-77–phosphorus-31 coupling constants are less in the complexes than in the free ligands and 1JPSe decreases in each observable case with decreasing temperature. Two bond mercury-199–phosphorus-31 coupling is observed in some of the cooled solutions of the complexes.