Synthesis and Characterization of Rhenium(V) Oxo Complexes with N-[N-(3-Diphenylphosphinopropionyl)glycyl]cysteine Methyl Ester. X-ray Crystal Structure of {ReO[Ph2P(CH2<
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- 作者：Roberta Visentin ; Raffaella Rossin ; Maria Cecilia Giron ; Alessandro Dolmella ; Giuliano Bandoli ; and Ulderico Mazzi
- 刊名：Inorganic Chemistry
- 出版年：2003
- 出版时间：February 24, 2003
- 年：2003
- 卷：42
- 期：4
- 页码：950 - 959
- 全文大小：148K
- 年卷期：v.42,no.4(February 24, 2003)
- ISSN：1520-510X
文摘
The PN2S chelate N-[N-(3-diphenylphosphinopropionyl)glycyl]-S-tritylcysteine methyl ester [PN2S(Trt)-OMe] wassynthesized and reacted with ReOCl3(PPh3)2 and Ph4P[ReOCl4]. The reactions of both tritylated and detritylatedligands with ReVO precursors gave two diastereomers, 9a and 9b, of the ReO(PN2S-OMe) complex. The twoisomers, produced in a 1:1 molar ratio, are stable and do not interconvert. They were separated by reverse-phaseHPLC and characterized by NMR, FT-IR, and UV-visible spectroscopy and electrospray mass spectrometry. X-rayanalysis established for 9a the presence in the solid of the syn isomer. Compound 9a, C21H23N2O5PSRe, crystallizedfrom warm acetonitrile in the triclinic space group P
, a = 9.828(2) Å, b = 11.163(2) Å, c = 11.641(2) Å, 
=106.48(3)
, 
= 109.06(3), 
= 102.81(3), V = 1085.7(4) Å3, Z = 2. The PN2S coordination set is in theequatorial plane, and the complex shows a distorted square pyramidal coordination. The anti configuration assignedto 9b is consistent with all the available physicochemical data. Follow-up of the reaction of the detritylated ligandwith Ph4P[ReOCl4] in ethanol or acetonitrile indicated that the phosphorus atom of the chelate binds first to themetal and that this bond acts as the driving force for coordination.
, a = 9.828(2) Å, b = 11.163(2) Å, c = 11.641(2) Å, =106.48(3), = 109.06(3), = 102.81(3), V = 1085.7(4) Å3, Z = 2. The PN2S coordination set is in theequatorial plane, and the complex shows a distorted square pyramidal coordination. The anti configuration assignedto 9b is consistent with all the available physicochemical data. Follow-up of the reaction of the detritylated ligandwith Ph4P[ReOCl4] in ethanol or acetonitrile indicated that the phosphorus atom of the chelate binds first to themetal and that this bond acts as the driving force for coordination.