Spectroscopic Properties of Inorganic and Organometallic Compounds: Volume 33 (Specialist Periodical Reports, Band 33) - Hardcover

 
9780854044269: Spectroscopic Properties of Inorganic and Organometallic Compounds: Volume 33 (Specialist Periodical Reports, Band 33)

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Spectroscopic Properties of Inorganic and Organometallic Compounds provides a unique source of information on an important area of chemistry. Divided into sections mainly according to the particular spectroscopic technique used, coverage in each volume includes: NMR (with reference to stereochemistry, dynamic systems, paramagnetic complexes, solid state NMR and Groups 13-18); nuclear quadrupole resonance spectroscopy; vibrational spectroscopy of main group and transition element compounds and coordinated ligands; and electron diffraction. Reflecting the growing volume of published work in this field, researchers will find this Specialist Periodical Report an invaluable source of information on current methods and applications. Specialist Periodical Reports provide systematic and detailed review coverage in major areas of chemical research. Compiled by teams of leading experts in their specialist fields, this series is designed to help the chemistry community keep current with the latest developments in their field. Each volume in the series is published either annually or biennially and is a superb reference point for researchers. www.rsc.org/spr

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Spectroscopic Properties of Inorganic and Organometallic Compounds provides a unique source of information on an important area of chemistry. Divided into sections mainly according to the particular spectroscopic technique used, coverage in each volume includes: NMR (with reference to stereochemistry, dynamic systems, paramagnetic complexes, solid state NMR and Groups 13-18); nuclear quadrupole resonance spectroscopy; vibrational spectroscopy of main group and transition element compounds and coordinated ligands; and electron diffraction. Reflecting the growing volume of published work in this field, researchers will find this Specialist Periodical Report an invaluable source of information on current methods and applications. Specialist Periodical Reports provide systematic and detailed review coverage in major areas of chemical research. Compiled by teams of leading experts in their specialist fields, this series is designed to help the chemistry community keep current with the latest developments in their field. Each volume in the series is published either annually or biennially and is a superb reference point for researchers. www.rsc.org/spr

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Spectroscopic Properties of Inorganic and Organometallic Compounds Volume 33

A Review of the Literature Published up to late 1999

By G. Davidson

The Royal Society of Chemistry

Copyright © 2000 The Royal Society of Chemistry
All rights reserved.
ISBN: 978-0-85404-426-9

Contents

Chapter 1 Nuclear Magnetic Resonance Spectroscopy By B. E. Mann, 1,
Chapter 2 Nuclear Quadrupole Resonance Spectroscopy By K.B. Dillon, 192,
Chapter 3 Characteristic Vibrations of Compounds of Main Group Elements By G. Davidson, 211,
Chapter 4 Vibrational Spectra of Transition Element Compounds By G. Davidson, 260,
Chapter 5 Vibrational Spectra of Some Co-ordinated Ligands By G. Davidson, 306,
Chapter 6 Mössbauer Spectroscopy By S.J. Clark, J.D. Donaldson and L.K. Mehta, 373,
Chapter 7 Gas-phase Molecular Structures Determined by Electron Diffraction By D. W.H. Rankin and H.E. Robertson, 500,


CHAPTER 1

Nuclear Magnetic Resonance Spectroscopy

BY B.E. MANN


1 Introduction

Following the criteria established in earlier volumes, only books and reviews directly relevant to this chapter are included, and the reader who requires a complete list is referred to the Specialist Periodical Reports 'Nuclear Magnetic Resonance', where a complete list of books and reviews is given. Reviews which are of direct relevance to a section of this report are included in the beginning of that section rather than here. Papers where only 1H, 2H, 13C, 19F, and/or 31P NMR spectroscopy is used are only included when they make a non-routine contribution, but complete coverage of relevant papers is still attempted where nuclei other than these are involved. In view of the greater restrictions on space, and the ever growing number of publications, many more papers in marginal areas have been omitted. This is especially the case in the sections on solid-state NMR spectroscopy, silicon and phosphorus.

A number of reviews have also been published: 'The DFT route to NMR chemical shifts', 'Correlations between transition-metal NMR chemical shifts and reactivities', which contains 51V NMR data, 'Probing organometallic structure and reactivity by transition metal NMR spectroscopy', which contains 51V, 53Cr, 55Mn, 57Fe, 59CO, 91Zr, 103Rh, and 187Os NMR data 'NMR spin-lattice relaxation approaches to characterization of transition metal hydride complexes in solution', 'Applications of heteronuclear X,Y-correlation spectroscopy in organometallic and organoelement chemistry', 'Direct determination of quadrupolar and dipolar NMR correlation times from spin-lattice and spin-spin relaxation rates', 'Reducing the NMR line widths of quadrupolar nuclei by employing supercriticial solvents', 'Comparative solid state and solution NMR structural and dynamic studies on tetra-and higher-nuclearity transition metal carbonyl clusters', 'NMR studies of molecular recognition by metalloporphyrins', 'Quadrupolar metal ion NMR studies of metalloproteins', which contains 27Al, 43Ca, 45Sc, 51V, 69Ga, and 71Ga NMR data, 'NMR spectroscopic studies of I = 1/2 metal ions in biological systems', which contains 109Ag, 111Cd, 113Cd, and 199Hg NMR data, 'Electronic state of ultrafine particles suspended in liquid media', and 'The characterisation and use of polycation-exchanged bentonites'.

A number of papers have been published which are too broadly based to fit into a later section and are included here. Complexes of the C(SiMe3) 2-SiMe2NMe2 with lithium, aluminium, mercury and tin have been investigated by 7Li, 15N, 27Al, 29Si, 119Sn, and 199Hg NMR spectroscopy. The 17O NMR tensors, electric field gradients and chemical shifts have been modelled in oxides and polyoxometallates. Density functional calculations of NMR chemical shifts have been applied to 183W and 207Pb chemical shifts in a wide range of compounds. A DFT-based study of 1K(M-X) has been reported for transition metal carbonyl, oxo, fluoro, and phosphine complexes. Line narrowing of I = 1/2 spins coupled to quadrupolar nuclei in liquids in the presence of weak decoupling fields has been examined and applied to 10B-enriched sodium borocaptate.


2 Stereochemistry

This section is subdivided into eleven parts which contain NMR information about Groups 1 and 2 and transition-metal complexes presented by Groups according to the Periodic Table. Within each Group, classification is by ligand type

2.1 Complexes of Groups 1 and 2 – Two reviews entitled 'Cryptand ligands for selective lithium coordination', which contains 7Li NMR data, and 31P NMR spectroscopy of the mouse heart', which contains 23Na NMR data, have appeared.

1J(13C6Li) has been observed in [Prn8(PrnO)4Li12]. The structure of Z-[(2,4, 6-But3C6 H2P=C)ClLi(sol)n,] has been determined using two-dimensional 31P, 6Li HMQC. 6Li and 15N NMR spectroscopy has been used to study [Et2NLi] solvated by oxetane, THF, and Et2O. NMR data have also been reported for [Li{CH(SiMe3)PPh2=NSiMe3} (OEt2)2], (7Li), lithiated allylic norbornenyl carbanions, (6Li), [ButSi(OSiMe2 NLiBut)3], [But(OSiMe2NH -SiMe3)3], (7Li, 15N, 29Si), [Ph2PNLiBut]2, (7Li), [MC(SiMe3)(SiMe2X)2], (M = Li, K; 7Li, 15N, 29Si), [LiC(SiMe2H) 3]·2THF, (7Li, 29Si), [ButO2 CCMe-LiCH2CMe2CO2But], (7Li), lithiated phosphoric triamides, (7Li), [Li{η3-CH-(CHSiMe2But)(CHSiMe2R)} (TMEDA)], (7Li, 29Si), [(HMe2Si)2 C=C(SiHMe2)2]-[MLn], (M = Li, Na, K, Rb, Cs; 6Li, 29Si), [Li{η3-PhCHCHCHCH(Boc) -C6H4-4-OMe}], (6Li), [Li2Ge C4Et4], (7Li), [Li3{1,2-(2,4,6 -C6H2)2-1,2-B2-3,5-Me2 -4-CH(SiMe3)2-C3}], (7Li, 11B), [Li2((C5Me4)SiMe2PCy}], (7Li), [Li(THF)4][2,6-(2,4,6-Me3C6H2)2 C6H3Cu2I2], (7Li) [Pri3SiSiLi2SiPri3], (6Li, 29Si), [Li(THF)3Sn(SiMe3) 3], (7Li, 29Si, 119Sn), (1), (7Li, 14N), side arm effects on cyclen-alkali metal cation complexation, (7Li, 23Na), (2), (7Li, 29Si), [LiNMe(CH2)2NMe2], (7Li), [(Me2NCH2CH2NMe)Li(THF)2], (6Li), [{Me2NCH2CMe2CH2N(H)Li}6], (6Li), [Li3{RNC(H)NC(H)NR)3], (7Li), [Pb(η5-P3C2But2) (μ-Cl)2Li(tmen)2], (7Li, 207Pb), [Li{N(SiMe2R1)-CBut(CH3)SiMe2 R2}(TMEDA)], (7Li, 29Si), (3), (7Li), Li+ complexes of (4), (7Li), [Li(R1 NSCR2)]n, (7Li), [(Pri3 SIP)10Li16], (7Li, 29Si), [LiPHB-(NPri2){N(SiMe3)2}], (7Li, 11B), and [Li(M[Te(NBUt)3] 2}], (M = Sb, Bi; 7Li, 125Te).

1H and 7Li magnetic relaxation dispersion data have been presented for the field dependence of T1 of [Me4N]+ and [Li(OH2)n]+ in GdIII and MnII solutions. 7Li double quantum filtered NMR spectra have been used to investigate ordering processes of synthetic Li+-saponites dispersed in water. The conformational behaviour of aqueous micelles of Na N-dodecanoyl-L-prolinate has been studied using 1H, 13C and 23Na NMR spectroscopy. Colloidal dispersions of sodium and potassium phosphates have been studied using 31P NMR spectroscopy. 87Rb NMR spectroscopy has been used to study molten and glassy 2Ca(NO3)2·3RbNO3. The 133Cs NMR spectrum of [NEt4][CS((η5 -C5Me5)Rh(CN)3}4{Mo(CO)3} 4] shows two signals due to free and bound Cs+ when Cs+ is added. 133Cs NMR spectroscopy has been used to investigate anisotropic block copolymers. The formation of micelles and aggregates in D2O solutions of [CnF2n+1 CO2Cs] has been studied using 19F and 133Cs NMR spectroscopy. NMR data have also been reported for [(Cy7 -Si7O12){Cy7Si7O11, (OSiMe3)}YLi2(THF)2(MeCN)], (29Si), [Li4(THF)4][(5)], (6Li, 29Si), [Li4(THF)4Mg{O2S(NBut)2} 3]2, (7Li), and [Li(diglyme)2][ (1,4-R2C8H6)2Sm2 (μ-Cl)3], (29Si).

7Li and 19F NMR spectroscopy has been used to study drugs in the brain. 7Li, 23Na, 87Rb and 31P NMR spectroscopy has...

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