화학공학소재연구정보센터
Inorganic Chemistry, Vol.33, No.6, 1184-1187, 1994
Transition-Metal Chemistry of Main-Group Hydrazides .5. Functionalization of Methylhydrazine with Alkyl Alkoxy Groups and Aryl Aryloxy-Substituted Phosphorus(V) Oxides and Sulfides - 1st Examples of Bidentate Interactions of R2P(E)(Nmenh2) (R=ome, OEt, OPh, pH E=s, O) with Pd(II) - X-Ray Structure of (Meo)2P(S)Nmenh2Pdcl2
The reactions of alkoxy-, aryloxy-, and aryl-substituted phosphorus monochlorides (R2P(E)Cl : R = OCH3, E = S; R = OC2H5, E = S; R = OC6H5, E = O; R = C6H5, E = O) with methyl hydrazine yielded the new monophosphorus hydrazides (R2P(E)NMeNH2 : R = OCH3, E = S (1); R = OC2H5, E = S (2), R = OC6H5, E = 0 (3); R = C6H5, E = O (4)) in good yields. The monophosphorus hydrazides 1-4 reacted smoothly with PdCl2(PhCN)2 at 25-degrees-C to give the new cyclopalladaphosphohydrazides R2P(E)NMeNH2.PdCl2 (R = OCH3, E = S (5); R = OC2H5, E = S (6); R = OC6H5, E = O (7); R = C6H5, E = O (8)) in good yields as air-stable crystalline solids. The chemical constitutions of 1-4 and 5-8 were established by complete NMR (H-1 and P-31) spectroscopic and C, H, N, and Cl analysis data. The structure of 5 was further confirmed by X-ray diffraction study. Crystal data for 5 : monoclinic, space group C2/c, with a = 25.029(9) angstrom, b = 10.2800(10) angstrom, c = 9.167(3) angstrom, beta = 104.750(10)-degrees, and Z = 8. The structure was solved by direct methods and was refined to R = 0.035.