C-13 CROSS-POLARIZATION MAGIC ANGLE SPINNING AND H-2 NMR-STUDIES OF THE STRUCTURE AND DYNAMICS OF THE (DEOXYCHOLIC ACID)2-FERROCENE INCLUSION COMPOUND

被引:11
作者
HEYES, SJ
DOBSON, CM
机构
[1] Inorganic Chemistry Laboratory, University of Oxford, Oxford, OX1 3QR, South Parks Road
关键词
!sup]13[!/sup]C CP/MAS NMR; !sup]2[!/sup]H NMR; (Deoxycholic acid)[!sub]2[!/sub]‐ferrocene; Dynamics; Inclusion compounds; Libration; Relaxation data; Reorientation;
D O I
10.1002/mrc.1260281309
中图分类号
O6 [化学];
学科分类号
0703 ;
摘要
The channel‐type inclusion complex, (deoxycholic acid)2–ferrocene [(DCA)2–;ferrocene], was studied by 13C cross‐polarization/magic angle spinning NMR spectroscopy. The spectra indicate that two different DCA molecules are present in the crystalline structure. Relaxation data indicate a relatively restricted degree of reorientational freedom of the included ferrocene molecules. 2H NMR spectra of the inclusion complex with perdeuterated ferrocene reveal rapid, anisotropic librations of the principal axes of the ferrocene molecules about their mean positions, varying from <ca. ± 1° at 160 K to ca. ± 28° at 350 K. The anisotropic, librational nature of this molecular reorientation may be rationalized in terms of the packing features of the sheet‐like nature of the structures of such deoxycholic acid compounds. Copyright © 1990 John Wiley & Sons, Ltd.
引用
收藏
页码:S37 / S46
页数:10
相关论文
共 32 条
[1]   CROSS POLARIZATION AND MAGIC ANGLE SAMPLE SPINNING NMR-SPECTRA OF MODEL ORGANIC-COMPOUNDS .3. EFFECT OF THE C-13-H-1 DIPOLAR INTERACTION ON CROSS POLARIZATION AND CARBON-PROTON DEPHASING [J].
ALEMANY, LB ;
GRANT, DM ;
ALGER, TD ;
PUGMIRE, RJ .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1983, 105 (22) :6697-6704
[2]   CROSS POLARIZATION AND MAGIC ANGLE SAMPLE SPINNING NMR-SPECTRA OF MODEL ORGANIC-COMPOUNDS .1. HIGHLY PROTONATED MOLECULES [J].
ALEMANY, LB ;
GRANT, DM ;
PUGMIRE, RJ ;
ALGER, TD ;
ZILM, KW .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1983, 105 (08) :2133-2141
[3]   ON THE NUCLEAR MAGNETIC RESONANCE IN METALS AND ALLOYS [J].
BLOEMBERGEN, N ;
ROWLAND, TJ .
ACTA METALLURGICA, 1953, 1 (06) :731-746
[4]   SPECTRAL DISTORTION EFFECTS DUE TO FINITE PULSE WIDTHS IN DEUTERIUM NUCLEAR MAGNETIC-RESONANCE SPECTROSCOPY [J].
BLOOM, M ;
DAVIS, JH ;
VALIC, MI .
CANADIAN JOURNAL OF PHYSICS, 1980, 58 (10) :1510-1517
[5]   H-2 NMR-STUDIES OF METALLOCENES IN HOST LATTICES [J].
CLAYDEN, NJ ;
DOBSON, CM ;
HEYES, SJ ;
WISEMAN, PJ .
JOURNAL OF INCLUSION PHENOMENA, 1987, 5 (01) :65-68
[6]  
CRAVEN BM, 1972, J CHEM SOC CHEM COMM, P530, DOI 10.1039/c39720000530
[7]   QUADRUPOLAR ECHO DEUTERON MAGNETIC-RESONANCE SPECTROSCOPY IN ORDERED HYDROCARBON CHAINS [J].
DAVIS, JH ;
JEFFREY, KR ;
BLOOM, M ;
VALIC, MI ;
HIGGS, TP .
CHEMICAL PHYSICS LETTERS, 1976, 42 (02) :390-394
[8]  
Fieser L.F., 1959, STEROIDS, p[53, 341]
[9]  
Giglio E., 1984, INCLUSION COMPOUNDS, V2, P207
[10]   SOLID-STATE C-13 NMR DETECTION OF A PERTURBED 6-S-TRANS CHROMOPHORE IN BACTERIORHODOPSIN [J].
HARBISON, GS ;
SMITH, SO ;
PARDOEN, JA ;
COURTIN, JML ;
LUGTENBURG, J ;
HERZFELD, J ;
MATHIES, RA ;
GRIFFIN, RG .
BIOCHEMISTRY, 1985, 24 (24) :6955-6962