A nuclear magnetic resonance method is presented which produces linear, isotropic proton-detected local-field spectra for INS spin systems in powdered samples. The method, heteronuclear isotropic evolution (HETIE), refocuses the anisotropic portion of the heteronuclear dipolar coupling frequencies by evolving the system under a series of specially designed Hamiltonians and evolution pathways. The theory behind HETIE is presented along with experimental studies conducted on a powdered sample of ferrocene, demonstrating the methodology outlined in this paper. Applications of HETIE for use in structure determination in the solid state are discussed.

1.
D. E.
Wemmer
,
Methods Enzymol.
309
,
536
(
1999
).
2.
D. D.
Laws
,
H. M. L.
Bitter
,
K.
Liu
 et al,
Proc. Natl. Acad. Sci. U.S.A.
98
,
11686
(
2001
).
3.
J.
van Beek
,
L.
Beaulieu
,
H.
Schafer
,
M.
Demura
,
T.
Asakura
, and
B.
Meier
,
Nature (London)
405
,
1077
(
2000
).
4.
R.
Tycko
,
Prog. Nucl. Magn. Reson. Spectrosc.
42
,
53
(
2003
).
5.
R. H.
Havlin
and
R.
Tycko
,
Proc. Natl. Acad. Sci. U.S.A.
(submitted).
6.
J. M.
Griffiths
and
R. G.
Griffin
,
Anal. Chim. Acta
283
,
1081
(
1993
).
7.
D. P.
Weitekamp
,
A.
Bielecki
,
D. B.
Zax
,
K.
Zilm
, and
A.
Pines
,
Phys. Rev. Lett.
50
,
1807
(
1983
).
8.
D. B.
Zax
,
A.
Bielecki
,
K. W.
Zilm
,
A.
Pines
, and
D. P.
Weitekamp
,
J. Chem. Phys.
83
,
4877
(
1985
).
9.
R.
Tycko
,
J. Magn. Reson. (1969-1992)
75
,
193
(
1987
).
11.
R.
Tycko
,
J. Chem. Phys.
92
,
5776
(
1990
).
12.
B. Q.
Sun
and
A.
Pines
,
J. Magn. Reson., Ser. A
109
,
157
(
1994
).
13.
M.
Hong
,
K.
Schmidt-rohr
, and
A.
Pines
,
J. Am. Chem. Soc.
117
,
3310
(
1995
).
14.
S.
Caldarelli
,
M.
Hong
,
L.
Emsley
, and
A.
Pines
,
J. Phys. Chem.
100
,
18696
(
1996
).
15.
D.
McElheny
,
E.
DeVita
, and
L.
Frydman
,
J. Magn. Reson.
143
,
321
(
2000
).
16.
J.
Grinshein
,
C. V.
Grant
, and
L.
Frydman
,
J. Am. Chem. Soc.
124
,
13344
(
2002
).
17.
J. D.
Walls
,
W. B.
Blanton
,
R. H.
Havlin
, and
A.
Pines
,
Chem. Phys. Lett.
363
,
372
(
2002
).
18.
U.
Haeberlen
and
J. S.
Waugh
,
Phys. Rev.
175
,
453
(
1968
).
19.
J. S.
Waugh
,
L. M.
Huber
, and
U.
Haeberlen
,
Phys. Rev. Lett.
20
,
180
(
1968
).
20.
M.
Carravetta
,
M.
Eden
,
X.
Zhao
,
A.
Brinkmann
, and
M. H.
Levitt
,
Chem. Phys. Lett.
321
,
205
(
2000
).
21.
Y. K.
Lee
,
N. D.
Kumur
,
M.
Helmle
,
O. G.
Johannessen
,
N. C.
Nielsen
, and
M. H.
Levitt
,
Chem. Phys. Lett.
242
,
304
(
1995
).
22.
C. P.
Brock
and
Y.
Fu
,
Acta Crystallogr., Sect. B: Struct. Sci.
B53
,
928
(
1997
).
23.
D.
Braga
,
Chem. Rev. (Washington, D.C.)
92
,
633
(
1992
).
24.
H. W.
Spiess
,
H.
Zimmermann
, and
U.
Haeberlen
,
Chem. Phys.
12
,
123
(
1976
).
25.
M.
Linder
,
A.
Hohener
, and
R. R.
Ernst
,
J. Chem. Phys.
73
,
4959
(
1980
).
26.
A.
Ramamoorthy
,
C.
Wu
, and
S.
Opella
,
J. Magn. Reson., Ser. B
107
,
88
(
1995
).
27.
A.
Ramamoorthy
and
S. J.
Opella
,
Solid State Nucl. Magn. Reson.
4
,
387
(
1995
).
28.
K. T.
Mueller
,
B. Q.
Sun
,
G. C.
Chingas
,
J. W.
Zwanziger
,
T.
Terao
, and
A.
Pines
,
J. Magn. Reson. (1969-1992)
86
,
470
(
1990
).
29.
P.
Madhu
,
X.
Zhao
, and
M.
Levitt
,
Chem. Phys. Lett.
346
,
142
(
2001
).
30.
A.
Brinkmann
,
M.
Eden
, and
M. H.
Levitt
,
J. Chem. Phys.
112
,
8539
(
2000
).
31.
The receiver phases in Fig. 4 of
Walls
 et al (Ref. 17) describing the HOMIE method is off by a minus sign in pathways X1, X2, Y1, Y2. The correct receiver phases (and the ones actually used) for the HOMIE method are the same as those shown in this figure.
32.
M.
Bak
,
J. T.
Rasmussen
, and
N. C.
Nielsen
,
J. Magn. Reson.
147
,
296
(
2000
).
You do not currently have access to this content.