31P and 13C NMR of Transition Metal Phosphine Complexes

31P and 13C NMR of Transition Metal Phosphine Complexes

Author: Paul S. Pregosin

Publisher: Springer Science & Business Media

Published: 2012-12-06

Total Pages: 164

ISBN-13: 3642488307

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For almost a quarter of a century the words "nuclear magnetic reso nance" were synonymous with proton I,leasurements. During this period the literature abounded with a seemingly infinite variety of 1H NHR studies concerned primarily with carbon chemistry. Occasionally a "novel" nucleus was studied and, even in those early days, the poten- 13 14 31 19 tial offered by C, N, P and F was clearly recognized. Despite the allure, the technical difficulties involved in measuring some of these nuclei were far from trivial. Small magnetic moments and low natural abundance in combination with spin-spin coupling from other nuclei, mostly protons, resulted in a signal-to-noise problem whose severity effectively excluded the study of metal complexes with unfa vorable solubility characteristics. The first important breakthrough came with the advent of broad band 1H-decoupling. For example, the featureless broad 31p resonance associated with the commonly used ligand triphenyl phosphine is converted to a sharp, more readily ob served singlet when wide-band decoupling is employed (see Fig. 1). Despite this improvement investigation of more interesting molecules, such as catalytically active complexes was forced to await the devel opment of Fourier Transform methods since only with relatively rapid signal averaging methods could sufficient signal-to-noise ratios be achieved.


Phosphorus-31 NMR Spectroscopy

Phosphorus-31 NMR Spectroscopy

Author: Olaf Kühl

Publisher: Springer Science & Business Media

Published: 2008-08-22

Total Pages: 138

ISBN-13: 3540791183

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Nuclear Magnetic Resonance is a powerful tool, especially for the identification of 1 13 hitherto unknown organic compounds. H- and C-NMR spectroscopy is known and applied by virtually every synthetically working Organic Chemist. Con- quently, the factors governing the differences in chemical shift values, based on chemical environment, bonding, temperature, solvent, pH, etc. , are well understood, and specialty methods developed for almost every conceivable structural challenge. Proton and carbon NMR spectroscopy is part of most bachelors degree courses, with advanced methods integrated into masters degree and other graduate courses. In view of this universal knowledge about proton and carbon NMR spectr- copy within the chemical community, it is remarkable that heteronuclear NMR is still looked upon as something of a curiosity. Admittedly, most organic compounds contain only nitrogen, oxygen, and sulfur atoms, as well as the obligatory hydrogen and carbon atoms, elements that have an unfavourable isotope distribution when it comes to NMR spectroscopy. Each of these three elements has a dominant isotope: 14 16 32 16 32 N (99. 63% natural abundance), O (99. 76%), and S (95. 02%), with O, S, and 34 14 S (4. 21%) NMR silent. N has a nuclear moment I = 1 and a sizeable quadrupolar moment that makes the NMR signals usually very broad and dif cult to analyse.


Handbook of Phosphorus-31 Nuclear Magnetic Resonance Data (1990)

Handbook of Phosphorus-31 Nuclear Magnetic Resonance Data (1990)

Author: John C. Tebby

Publisher: CRC Press

Published: 2017-11-22

Total Pages: 582

ISBN-13: 1351362046

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To fully utilize Nuclear Magnetic Resonance (NMR) spectroscopy, a comprehensive and well-organized compilation of NMR data is necessary. While compilations have been available for other important NMR nuclei, such as carbon and fluorine, no comprehensive collection of data has been prepared for phosphorus-until now. The CRC Handbook of Phosphorus-31 Nuclear Magnetic Resonance Data provides a collection of 31P NMR chemical shifts for nearly 20,000 organic and inorganic phosphorus compounds. Each class of phosphorus compound is discussed. Bond types, stereochemistry (with the exception of metal complexes), media, important coupling constants, and data sources are included. The information is systematically organized according to coordination state, the atoms bound to phosphorus, and their connectivities. A comprehensive series of bar charts is also included to allow structure types to be assigned to chemical shift data. This handbook is an invaluable resource for all scientists working with phosphorus compounds, including chemists, biochemists, medical researchers, and pharmaceutical chemists.


Phosphorus Coordination Compounds of Transition Metals

Phosphorus Coordination Compounds of Transition Metals

Author: Samuel O. Grim

Publisher:

Published: 1967

Total Pages: 43

ISBN-13:

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The phosphorus-31 nmr spectra of eleven cis and seven trans compounds of the type (R sub n Ph sub 3-n P)2PtCl2, where R = alkyl and n = 1,2, or 3, show that the platinum-195 to phosphorus-31 coupling constant is always larger for the cis compound than for the corresponding trans compound and that the phosphorus chemical shift of the cis compound is upfield from that of the corresponding trans compound. The formation of the tris-phosphine complex by addition of excess tertiary phosphine to the monomer has been demonstrated by conductivity and 31p nmr measurements and confirmed by isolation of the compounds, (MePh2P)3PtCl)Cl and (PrPh2P)3 - PtCl)BPh4. The preparation of several new chlorine bridged dimers is also reported. The phosphorus-31 chemical shifts are reported for twenty-five compounds of the type (RnPh sub 3-nP)M(CO)5, where R is alkyl, n is 0,1,2,3 and M is Cr, Mo, or W. The 183W-31P spin-spin coupling is observed for all the tungsten compounds and a linear correlation exists between these coupling constants and the carbonyl stretching frequencies in the respective compounds. (Author).


NMR.

NMR.

Author: Gérard J. Martin

Publisher:

Published: 1969

Total Pages: 402

ISBN-13:

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Handbook of Phosphorus-31 Nuclear Magnetic Resonance Data

Handbook of Phosphorus-31 Nuclear Magnetic Resonance Data

Author: John C. Tebby

Publisher: CRC Press

Published: 1990-12-26

Total Pages: 584

ISBN-13: 9780849335310

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To fully utilize Nuclear Magnetic Resonance (NMR) spectroscopy, a comprehensive and well-organized compilation of NMR data is necessary. While compilations have been available for other important NMR nuclei, such as carbon and fluorine, no comprehensive collection of data has been prepared for phosphorus-until now. The CRC Handbook of Phosphorus-31 Nuclear Magnetic Resonance Data provides a collection of 31P NMR chemical shifts for nearly 20,000 organic and inorganic phosphorus compounds. Each class of phosphorus compound is discussed. Bond types, stereochemistry (with the exception of metal complexes), media, important coupling constants, and data sources are included. The information is systematically organized according to coordination state, the atoms bound to phosphorus, and their connectivities. A comprehensive series of bar charts is also included to allow structure types to be assigned to chemical shift data. This handbook is an invaluable resource for all scientists working with phosphorus compounds, including chemists, biochemists, medical researchers, and pharmaceutical chemists.