Cinellu, Maria Agostina and Gladiali, Serafino Gabriele and Minghetti, Giovanni and Stoccoro, Sergio and Demartin, Francesco (1991) Cyclometallated derivatives of palladium(II) with 1,4-benzodiazepin-2-ones: crystal structure of (L-H)Pd(PPh3)Cl•CHCl3 (L = Prazepam: 7-chloro-1-cyclopropylmethyl-1,3-dihydro-5-phenyl-2H-1,4-benzodiazepin-2-one): synthesis of isoindolo[2,1-d][1,4]benzodiazepine derivatives by reaction of [(L-H)PdCl]2 species with carbon monoxide. Journal of Organometallic Chemistry, Vol. 401 (3), p. 371-384. ISSN 0022-328X. Article.
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The dimeric cyclometallated derivatives of palladium(II) [(L-H)PdCl]2, 3 (L = 1, Diazepam: 7-chloro-1,3-dihydro-1-methyl-5-phenyl-2H-1,4-benzodiazepin-2-one) and 4 (L = 2, Prazepam: 7-chloro-1-cyclopropylmethyl-1,3-dihydro-5-phenyl-2H-1,4-benzodiazepin-2-one) react with triphenylphosphine to give the complexes (L-H)Pd(PPh3)Cl, 5(L = Diazepam) and 6 (L = Prazepam). The crystal structure of 6 was determined by X-ray crystallography. The palladium atom is in a square planar arrangement. The deprotonated ligand is bound to the metal through the 4-nitrogen and the ortho-carbon atom of the 5-phenyl substituent. The phosphorous and the chlorine atoms are trans to the nitrogen and the carbon atoms, respectively: Pd---N = 2.085(2), Pd---P=2.263(1), Pd---Cl = 2.377(1), Pd---C = 2.009(3) Å.
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