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Abstract
The reaction of 1-methyl-2-chloro-3-dichlorophosphinyl-1,3,2λ3-diazaphosphorinane 1 with (norbornadiene)tetracarbonylmolybdenum(0) in a 2:1 molar ratio furnished cis-bis(1-methyl-2-chloro-3-dichlo-rophosphinyl-1,3,2-diazaphosphorinane)tetracarbonylmolybdenum(0) 2. In 2, one ligand 1 is bonded to Mo(0) via the Pcl group, the other through the Pl2 group. 1-Methyl-2-methoxy-3-dimethoxyphos-phinyl-1,3,2λ3-diazaphosphorinane 3 reacted with norbornadienetetracarbonyl-molybdenum(0) to form the chelate complex cis-(1-methyl-2-methoxy-3-dimethoxyphosphinyl-1,3,2-diazaphosphorinane)tetracarbonylmolybdenum(0) 4, in which one molecule of the ligand 3 is attached to Mo(0) in a chelating fashion, coordinating through both the POCH3 and the P(OCH3)2 group. In the reaction of 3 with (COD)PtCl2 (COD = 1,5-cyclooctadiene) in a 2:1 molar ratio the ionic bis-chelate complex cis-bis(1-methyl-2-methoxy-3-dimethoxyphosphinyl-1,3,2-diazaphosphorinane)-platinum(II)chloride 5 was formed. Two molecules of 3 are coordinated to Pt(II) in the same fashion as in 4. The characterization of 2, 4, 5 is based on their 1H-, 13C- and 31P-n.m.r.-spectra, and their mass spectra and infrared spectra. The structure of the chelate complex 4 was confirmed by a single-crystal X-ray structure analysis. The ligand 3 is coordinated via both phosphorus atoms; the four-membered ring has a very narrow “bite” angle of 64.08(3)°, and the molybdenum atom thus displays distorted octahedral coordination geometry. Both phosphorus atoms have strongly distorted tetrahedral coordination geometry. The six-membered heterocycle assumes a chair conformation.