Abstract Dihydrazido thiophosphoric acid phenyl ester, (NH2NH)2P(= S)-OC6H5 (DHTPPH), forms a 2:1 complex with manganese(II) chloride: [Mn(II)(DHTPPh)2Cl2], soluble in methanol. Solvolysis yields the corresponding methyl ester complex. With water in methanol the dihydrazidothiophosphato complex [Mn(II){(NH2NH)2P(= O)S}2] is formed. Monohydrazido thiophosphoric acid diphenyl ester NH2NH-P(= S)(OC6H5)2 (MHTPPh) gives various complexes with first row transition metals: [M(II)(MHTPPh)nX2], n = 2, 4; X = halogen. The nickel complex (n = 4; X = Cl) is characterized by elemental analysis and spectroscopic methods. MHTPPh is monodentate through the terminal N atoms of the hydrazido groups. Iron(II) and cadmium complexes have different compositions (n- 2; X = Cl) and therefore different structures, probably with MHTPPh as a bidentate chelate ligand.
Abstract The title compounds are prepared from trichloromethylphosphonic acid dichloride and excess hydrazine hydrate, and from the dihydrazide and the dichloride in the presence of triethylamine, resp. They are characterized by elemental analysis, mass spectra, 1H and 31P NMR spectra, IR and Raman data. Thin layer chromatographic experiments show that in the raw material of the ring compound two isomers (probably cis- and trans-) are present, whereas in the recrystallized product only one isomer can be detected. Attempts of a preparative separation of isomers were unsuccessfull so far due to very low concentrations of the product with the slightly higher Rf. Single crystals of the isolated ring compound decompose on irradiation with X-rays
Das Dihydrazid (II) wird durch Umsetzung des Phosphonsäuredichlorids (I) mit überschüssigem Hydrazinhydrat erhalten und bildet mit äquimolaren Mengen des Dichlorids (I) in Gegenwart von Triethylamin das cyclische Produkt (III).
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