Gas and Liquid Phase Diffusivities of Isomeric Metal Complexes Derived from Multifold Ring-Closing Metatheses: Ion Mobility Mass Spectrometry Trumps DOSY NMR

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• 作者：Tobias Fiedler ; Liuxi Chen ; Nicole D. Wagner ; David H. Russell ; John A. Gladysz
• 刊名：Organometallics
• 出版年：2016
• 出版时间：June 27, 2016
• 年：2016
• 卷：35
• 期：12
• 页码：2071-2075
• 全文大小：429K
• 年卷期：0
• ISSN：1520-6041

文摘

Isomeric octahedral osmium and rhenium complexes of formulas M(CO)_y(X)_z(P((CH₂)_n)₃P) and M(CO)_y(X)_z(P(CH₂)_n−1CH₂)((CH₂)_n)(P(CH₂)_n−1CH₂) (n/M/y/z/X = 14/Os/2/2/Cl, 14/Os/2/2/Br, 14/Re/3/1/Cl, 18/Os/2/2/Br), in which the phosphorus donor atoms occupy trans positions, are examined by the title techniques. The former gyroscope-like complexes are spherical or ovoid in shape, whereas the latter have phosphacycle “flaps” that increase the volume. Both types diffuse at identical rates in C₆D₆ as assayed by DOSY NMR, but ions derived from the latter exhibit up to 10% slower drift times in the gas phase by ion mobility mass spectrometry (IMMS). Thus, IMMS, which is seldom applied to isomeric organometallic or coordination compounds, provides superior differentiation.