MEASUREMENT OF CHEMICAL SHIELDING TENSOR

Abstract

Abstract:

In rigid lattice, chemical shift is a tensor depending on the spatial orientation of the external magnetic field. The tensor has six independent components. The orientation of chemical shielding tensor can be expressed with direction cosine s of its principal axis system. It is of great interest that if the chemical shi ft tensor of each nonmagnetically equivalent nucleus is known, the information o n the distribution of the electron cloud in the molecule can be deduced from the se tensors. In this paper, the theory and methods of measurement of chemical shi ft tensor are reviewed. A number of common methods are discussed in detail, such as 2D magic angle hopping (MAH), 2D magic angle turning(MAT), and 2D phase-adjusted spinning sidebands(2D-PASS) technique and so on. The common metho ds for measuring single crystal chemical shielding tensor are also discussed.

Key words: chemical shift anisotropy (CSA) tensor, magic angle hopping (MAH), ma gic angle turning (MAT), 2D-PASS

CLC Number:

O482.53

WANG Li-ying, DENG Feng, YE Chao-hui*. MEASUREMENT OF CHEMICAL SHIELDING TENSOR[J]. Chinese Journal of Magnetic Resonance.

References

[1] Mehring M. Pinciples of High Resolution NMR Solids[M]. 2nd ed. New York: Spri nger Verlag, 1983.25-30.

[2] Haeberlen U. High resolution NMR in Solids, selective averaging[M]. New York: Academic Press, 1976.

[3] Hohwy M, Rasmussen J T, Bower P V, et al. ¹H Chemica l Shielding Anisotroscopies from Polycrystalline Powder Using MSHOT₃ Based CRA MPS[J]. J Magn Reson, 998,133:374-378.

[4] Hughes E, Brouwer E B, Harris R K. Fluorine-19 Solid-State NMR Magi c-Angl e-Turning Experiments Using Multiple-Pulse Homonuclear Decoupling[J]. J Magn Reson, 1999,138:256.

[5] Lippmaa E, Alla M, Tuherm T. Proc 19th. Ampere Congress[C]. Heideberg 1 976,113.

[6] Bax Ad, Szeverenyi N M, Maciel G E. Chemical Shift Anisotropy in Powd ered Solids Studied by 2D FT CP/MAS NMR[J]. J Magn Reson, 1983,51:400-408.

[7] Stejskal E O, Schaefer J, Mckay R A. High-Resolution Slow-Spinning M agic-Angle Carbon-13 NMR[J]. J Magn Reson, 1977,25:569.

[8] Sethi N K, Grant D M, Pugmire R J.¹³C Chemical Shielding A nisot ropy Studied by Variable-Angle Sample Spinning[J]. J Magn Reson, 1987,71:476- 479.

[9] Maricq M M, Waugh J S. NMR in Rotating Solids[J]. J Chem Phys, 1979,70: 3300.

[10] Dixon W T. Spinning-Sideband-Free NMR Spectra[J]. J Magn Reson , 1981,44:220.

[11] Dixon W T. Spinning-sideband-free and Spinning-sideband-only NMR Spe ctra in spinning samples[J]. J Chem Phys, 1982,77:1800.

[12] Herzfield J, Berger A E. Sideband intensities in NMR spectra of samp les spinning at the magic angle[J]. J Chem Phys, 1980,73:6021.

[13] Bax Ad, Szeverenyi N M, Maciel G E. Correlation of Isotropic Shifts and Chemical Shift Anisotropies by Two-Dimensional Fourier-Fransform Magic-Angle Hopping NMR Spectroscopy[J]. J Magn Reson,1983,52:147-152.

[14] Gan Z. High-Resolution Chemical Shift and Chemical Shift Anisotropy cor rela tion in Solids Using Slow Magic Angle Spinning[J]. J Am Chem Soc, 1992,114:830 7-8310.

[15] Gan Z. Spinning-Sideband Suppression Using a Peseudo-Two-Dimensional Experiment[J]. J Magn Reson, 1994,109A:253-255.

[16] Hu J Z, Alderman D W, Ye C, et al. An Isotropic Chemica l Shift-Chemical Shift Anisotropy Magic-Angle Slow-Spinning 2D NMR Experiment[J]. J Magn Reson, 1993,A105:82-87.

[17] Kolbert A C, Griffin R G. Two-Dimensional Resolution of Isotropic a nd An isotropic Chemical Shifts in Magic Angle Spinning NMR[J]. Chem Phys Lett, 1990 ,166:87-91.

[18] Hu J Z, Orendt A M, Alderman D W, et al. Measurem ent of ¹³C Chemical Shift Tensor Principal Values with a Magic-Angle Turning Experiment[J]. Solid State Nucl Magn Reson, 1994,3:181-197.

[19] Hu J Z, Wang W, Liu F, et al. Magic-Angle-Turning Experimen ts ofr Measuring Chemical-Shift-Tensor Principal Values in Powdered Solids[J]. J Magn Reson, 1995,A113:210-222.

[20] Antzatkin Oleg N, Shekar S C, Levitt Malcolm H. Two-Dimensional Sid eband Separation in Magic-Angle-Spinning NMR[J]. J Magn Reson, 1995,A115:7-9 .

[21] de Lacroix S F, Titman J J, Hagemeyer A, et al. Increased Resolutio n in MAS NMR Spectra by Two-Dimensional Separation of Sidebands by Order[J].J Magn Reson, 1992,97:435-443.

[22] Crockford C, Geen H, Titman J J. Two-dimensional MAS-NMR spectra which corr elate fast and slow magic angle spinning sideband patterns[J].Chem Phts Lett , 2001,344:367-373.

[23] Zeigler R C, Wind R A, Maciel G E. The Stop and Go Spinning Techniqu e in MAS Experiments[J]. J Magn Reson, 1988,79:299-306.

[24] Kolbert A C, M DeGroot H J, Griffin R G. Two-Dimensional Switched- Speed Spinning NMR[J]. J Magn Reson, 1989, 85:60-68.

[25] Terao T, Fujii T, Onodera T, et al. Switching-Angle Sample-Spinni ng NM R Spectroscopy for Obtaining Powder-Pattern-Resolved 2D Spectra: Measurements of ¹³C ChemicalShift Anisotropies in Powdered 3,4-Dimethoxybenzaldehy de[J]. Chem Phys Lett, 1984,107:145-148.

[26] Frydman L, Chingas G C, Lee Y K, et al. Variable-Angle Correlation Spectros copy in SolidState Nuclear Magnetic Resonance[J]. J Chem Phys，1992, 97:4800 -4808.

[27] Frydman L, Chingas G C, Lee Y K, et al. Isr J Chem[J], 1992,32:16 1.

[28] Gullion T. Extended Chemical-Shift Modulation[J]. J Magn Reson, 1989, 85:614-619.

[29] Gullion T, Poliks M D, Schadfer J. Extended Dipolar Modulation and M agic-Angle Spinning[J]. J Magn Reson, 1988,80:553-558.

[30] Hughes C D, Sherwood M H, Alderman D W, et al. Chemical-Shift-Chemical-Shift Correlation Spectroscopy in Powdered Solids[J]. J Magn Reson, 1993,A 102:58-72.

[31] 胡建治. 固态NMR新技术的发展与应用\[D\]. 武汉:中国科学院武汉物理研究所, 1 994.

[32] Linder M, Hohener A, Ernst R R. Orientation of Tensorial Interactions Determined from Two-Dimensional NMR Powder Spectra[J]. J Chem Phys, 1980,73( 10):4959.

[33] Hester R K, Alderman J L, Neff B L, et al. Quantum Motion of Ch emisorbed Hydrogen on Ni Surfaces[J]. Physical Rev lett, 1983,36(18):1081.

[34] Rybaczewski E F, Neff B L, Waugh J S, et al. High Resolution ¹³C NMR in Solids: ¹³C Local Fields of CH, CH₂ and CH₃[J]. J Ch em Phys, 1977,67(3):1231.

[35] Arun Kumar B S, Opella S J. Three-Dimensional Sideband Separated-Local-Field/Dilute-Spin-Exchange Solid-State NMR Spectrascopy[J]. J Magn Reson, 19 93,A101:333-336.

[36] Zilm K W, Webb G G, Cowley A H, et al. The Nature of t he Phosphorus-Phosphorus Double Bond As Studied by Solid-State NMR[J]. J Am Chem Soc, 1988,110:2032.

[37] Nakai T, McDowell C A. Residual Chemical-Shift Effects in Spin-echo NMR Powder Patterns of Homonuclear Dipolar-coupled Spins[J]. Chem Phys Lett, 1994 ,217:234.

[38] Nakai T, McDowell C A. Characterization of Homonuclear Spin Pairs fr om Two-Dimensional Spin-Echo NMR Powder Patterns[J]. J Am Chem Soc, 1994,116 :6373.

[39] Nakai T, McDowell C A. Determination of Spin Parameters Reflected in the Nuclear Magnetic Resonance Powder Patterns for Two Equivalent ³¹P Nuc lei in Lawessen's Reagent[J]. Solid State NMR, 1995,4:163.

[40] Ashida J, Nakai T, Terao T. 1D NMR Separation of overlapping Powder Patt erns by Selective RF Irradiation and Switching-Angle Spinning[J]. Chem Phys L ett, 1990,168:523.

[41] Teras T, Miura H, Saika A. Dipolar SASS NMR Spectroscopy: Separation of Heteronuclear Dipolar Powder Patterns in Rotating Solids\[J\]. J Chem Phys, 1986 ,85:3816.

[42] Nakai T, Ashida J, Terao T. Measurements of TwoDimensional NMR Pow der Patterns in Totating Solids[J]. J Chem Phys, 1988,88:6049.

[43] Nakai T, Terao T, Shirakawa H. Determination of ¹³C Chemic al Shift Tensor Orientations in Cis and Trans-Polyacethylene by Measurements of Two-Dimensi onal NMR Powder Patterns in Rotating Solids[J]. Chem Phys Lett, 1988,145:90.

[44] Canet D, Barthe P, Mutzenhardt P, Roumestand C. A Comprehensive Analy sis of Multifield ¹⁵N Chemical Shift Anisotropies[J]. J Am Chem Soc, 2001,123:456 7-4576.

[45] Veeman W S. Carbon-13 Chemical Shift Anisotropy[J]. Prog NMR Spectrosc, 1984,16:193.

[46] Veeman W S. ¹³C Chemical Shift Tensors in Organic Single Cr ystals[J]. Phil Trans R Soc Lond, 1981,A299:629.

[47] Pines A, Abramson E. Chemical Shift Tensors of ¹³C in Sol id Dimethy Oxalate[J]. J Chem Phys, 1974,60:5130.

[48] Chang J J, Griffin R G, Pines A. Chemical Shift Tensors of ¹³C in a Carboxyl Group[J]. J Chem Phys, 1974,60:2561.

[49] Chang J J, Griffin R G, Pines A. Carbon-13 Chemical Shielding Tensor s in Ammonium Hydrogen Maloate[J]. J Chem Phys, 1975, 62:4923.

[50] Van J, Torman D, Veeman W S. Carbon-13 Chemical Shielding Tensors i n para-xylene[J]. J Chem Phys, 1978,68:3233.

[51] Pausak S, Pines A, Waugh J S. Carbon-13 Chemical Shielding Tensors in S ingle-Crystal Durene[J]. J Chem Phys, 1973,59:591.

[52] Takegoshi K, Naito A, Mcdowell C A. Intermolecular Hydrogen-Bonding-Effects on the ¹³C NMR Shielding Tensor of the Carbonyl Carbon Nucleus in a Single Crystal of Dimedene[J]. J Magn Reson, 1985,65:34.

[53] Mcdowell C A, Naito A, Saztry D L, et al.¹³C and ³¹P Chemical Shie lding Tensors of a Single Crystal of Dipotassium α-D-Glucose-1-Phosphate Di hydr ate an Application of a ¹³C-¹H, ³¹P Triple Resonance Techniq ue[J]. J Magn Reson, 1988,78:498.

[54] Naito A, Ganapathy S, Akasaka K, et al. Chemical Shielding Tensor and ¹³C-¹⁵N Dipolar Splitting in Single Crystals of L-alanine [J]. J Chem Phys, 1981,74:3190.

[55] Haberkorn R A, Stark R E, Willigen H van,

et al. Determination of Bond Distance and Bond Angles by Solid-State Nuclear Magnetic Resonance ¹³C and 15N NMR Study of Glycine[J]. J Am Chem Soc, 1981,103:2534.

[56] Janes N, Ganapathy S, Oldfield E. Carbon-13 Chemical Shielding Tens ors in L-Threonine[J]. J Magn Reson, 1983,54:111.

[57] Sastry D L, Takegoshi K, Mcdowell C A. Determination of the ¹³C Chemical -Shift Tensors in Single Crystal of Methyl α-D-Glucopyranoside[J]. Carboh ydr Res, 1987,165:161.

[58] Griffin R G, Ellet J D, Mehring M, et al. Two-Dimensiona l Nuclear Magnetic Resonance with Sample Flip for Characterizing Orientation Dis tributions and its Analogy to X-Ray Scattering[J]. J Chem Phys, 1992,57:2147.

[59] 孙伯勤. 旋转固体核磁共振行为的研究\[D\]. 武汉:中国科学院武汉物理所,1985.

[60] Carter C M, Alderman D W, Grant D M. Two-Dimensional Chemical-Shif t Anisotropy Correlation Spectroscopy[J]. J Magn Reson, 1985,65:183.

[61] Carter C M. Alderman D W, Grant D M. Two-Dimensional Chemical-Shift Anis otropy Correlation Spectroscopy Measurements in Complex Single Crystals[J]. J Magn Reson, 1987,73:114.

[62] 傅日强. 固体屏蔽张量测量的实验研究[D]. 武汉:中国科学院武汉物理所,1989.