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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Intrinsic Cl-37/35 and O-18/16 isotope shifts in Pt-195 and Rh-103 NMR of purely inorganic Pt and Rh complexes as unique spectroscopic fingerprints for unambiguous assignment of structure
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Intrinsic Cl-37/35 and O-18/16 isotope shifts in Pt-195 and Rh-103 NMR of purely inorganic Pt and Rh complexes as unique spectroscopic fingerprints for unambiguous assignment of structure

机译：固有Cl-37/35和O-18/16同位素在Pt-195和Rh-103 NMR中偏移，纯无机PT和RH复合物，作为唯一的光谱指纹，用于明确分配结构

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摘要

Well-resolved intrinsic (1)Delta M(Cl-37/35) and (1)Delta M(O-18/16) isotope shifts (where M = Pt-195 or Rh-103) are visible in the Pt-195 NMR peak profiles of relatively kinetically inert [PtCln(H2O)(6-n)](4-n) (n = 1-6) complexes, their corresponding hydroxido [PtCl6-n(OH)(n)](2-) (n = 1-5/6) anions, and [RhCln(H2O)(6-n)](3-n) (n = 3-6) complexes in aqueous solutions at ca. 293 K. Although some such isotope effects have been previously reported, there are very limited published data in the open literature, and the first systematic studies of such intrinsic (1)Delta M(Cl-37/35) and (1)Delta M(O-18/16) isotope effects are reviewed in this perspective. In high magnetic-field NMR spectrometers, the Pt-195 and Rh-103 NMR peak profiles acquired within a relatively narrow temperature range (288-300 K) constitute unique 'spectroscopic fingerprints', which allow unambiguous structural assignment in solution. Available data for Pt(IV) and Rh(III) complexes give rise to intrinsic isotope (1)Delta delta Pt-195/Rh-103(Cl-37/35) profiles, which are extraordinarily sensitive to the structure of a particular complex or its geometric isomer. The profiles of aquated Pt(IV) and Rh(III) complexes in acidic solutions may be resolved at either an isotopologue level only or at both an isotopologue and an isotopomer level depending on the structure. By contrast, in the series of [PtCl6-n(OH)(n)](2-) (n = 1-6) anions, (1)Delta delta Pt-195(Cl-37/35) isotope shifts are resolved only at an isotopologue level. Relatively larger (1)Delta Pt-195(O-18/16) isotope shifts obtained by the partial O-18 enrichment of both the [PtCln(H2O)(6-n)](4-n) (n = 1-6) and [PtCl6-n(OH)(n)](2) (n = 1-6) series give rise to remarkable Pt-195 NMR peak profiles showing both Cl-37/35 and O-18/16 shifts. In the [PtCl6-n(OH)(n)](2-) (n = 1-5/6) anions a typical NMR peak profile spanning similar to 2 ppm only may be resolved at both the isotopologue and isotopomer levels, depending on whether (OH)-O-18/16-ions are coordinated trans to chloride ions or not. The potential utility of such (1)Delta Pt-195(Cl-37/35) and (1)Delta Pt-195(O-18/16) isotope shifts in selected practical applications involving such complexes is briefly illustrated.
机译：分解的内在（1）ΔM（Cl-37/35）和（1）ΔM（O-18/16）同位素偏移（其中M = Pt-195或RH-103）在PT-195中可见相对动力学惰性的NMR峰谱[PTCLN（H2O）（6-N）]（4-N）（N = 1-6）络合物，它们相应的Hydroxido [PtCl6-N（OH）（N）]（2-） （n = 1-5 / 6）阴离子，[rhcln（h2O）（6-n）]（3-n）（3-n）（3-n）（n = 3-6）络合物在Ca的水溶液中。 293 K.虽然先前已经报道了一些这样的同位素效应，但公开文学中的公布数据非常有限，并且对这种内在（1）ΔM（CL-37/35）和（1）ΔM的第一系统研究（O-18/16）在此视角审查了同位素效应。在高磁场NMR光谱仪中，在相对较窄的温度范围内获得的PT-195和RH-103 NMR峰谱构成独特的“光谱指纹”，其允许在溶液中占据明确的结构分配。 Pt（IV）和RH（III）复合物的可用数据产生内在同位素（1）ΔδPT-195 / RH-103（CL-37/35）型材，这对于特定复合物的结构非常敏感或其几何异构体。酸性溶液中的水分Pt（IV）和Rh（III）复合物的谱可以在同位素水平或在同位素水平和同位素水平上根据结构分解。相反，在[Ptcl6-n（OH）（n）]（2-）（2-）（n = 1-6）阴离子的系列中，解析（1）Δδpt-195（cl-37/35）的同位素偏移只在同位素水平。相对较大（1）ΔPt-195（O-18/16）通过部分O-18富集[Ptcln（H2O）（6-N）]（4-N）（n = 1-）获得的同位素偏移6）和[PTCL6-N（OH）（N）]（2）（n = 1-6）系列产生显着的PT-195 NMR峰谱，显示CL-37/35和O-18/16偏移。在[PtCl6-N（OH）（N）]（2-）（n = 1-5 / 6）阴影中，仅在同位素和同位素水平的情况下，跨越类似于2ppm的典型NMR峰谱跨越的典型的NMR峰谱率无论是（OH）-O-18 / 16-离子是否配合到氯离子。简要介绍了涉及这些复合物的所选实际应用中的（1）ΔPT-195（CL-37/35）和（1）ΔPt-195（O-18/16）同位素的潜在效用。

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