Abstract: | Mixed‐ligands hydride complexes RuHCl(CO)(PPh3)2{P(OR)3}] ( 2 ) (R = Me, Et) were prepared by allowing RuHCl(CO)(PPh3)3] ( 1 ) to react with an excess of phosphites P(OR)3 in refluxing benzene. Treatment of hydrides 2 first with triflic acid and next with an excess of hydrazine afforded hydrazine complexes RuCl(CO)(κ1‐NH2NHR1)(PPh3)2{P(OR)3}]BPh4 ( 3 , 4 ) (R1 = H, CH3). Diethylcyanamide derivatives RuCl(CO)(N≡CNEt2)(PPh3)2{P(OR)3}]BPh4 ( 5 ) were also prepared by reacting 2 first with HOTf and then with N≡CNEt2. The complexes were characterized spectroscopically and by X‐ray crystal structure determination of RuHCl(CO)(PPh3)2{P(OEt)3}] ( 2b ). |