Supplementary Material for Chemical Communications
This journal is © The Royal Society of Chemistry 2003
Synthesis
magnesium
of
the
mixed
lithium-potassium-(bis)
N-metallated/N,C-dimetallated
amide
[Li2K2Mg4{But(Me3Si)N}4{But[Me2(H2C)Si]N4}]:
an
inverse crown molecule with an atomless cavity
Glenn C. Forbes, Fiona R. Kenley, Alan R. Kennedy, Robert
E. Mulvey, Charles T. O’Hara and John A. Parkinson
Supporting Information
i
Figure S1:
2D [1H, 13C] HSQC NMR spectrum acquired at a magnetic field
strength of 9.4 T and optimised for 1J(1H, 13C) = 136 Hz (1/4J = 1.8
ms). a) N-methyl region; b) Silyl-methyl region.
 10
b)
ppm
5
10
15
1
13
20
C (ppm)
25
30
a)
35
40
1.5
1.0
0.5
ppm
-1.5
2 – 1H (ppm)
-2.0 ppm
ii
2D [1H, 29Si] HSQC NMR spectrum acquired at a magnetic field
strength of 9.4 T and optimised for 2J(1H, 29Si) = 6.6 Hz (1/4J = 38
ms). a) 0.0-0.7 ppm (1H) region; b) Low ppm region indicating that the
signal at -1.9 ppm is associated with a CH2 group adjacent to 29Si (nonequivalent geminal protons giving rise to two signals with strong
coupling [large ‘roof effect’]). At this temperature the broad 1H
resonance at –1.5 ppm does not give rise to a correlation with 29Si.
Figure S2:
 10
ppm
1
29
a)
b)
-90
Si (ppm)
-80
-70
0.6
0.4
0.2
ppm
-1.5
-2.0 ppm
2 - 1H (ppm)
iii
Figure S3:
N-methyl region of the 1H 2D EXSY NMR spectrum acquired at a
magnetic field strength of 9.4 T (mixing time = 500 ms). 1D 1H NMR
spectra of the same regions are shown as projections (top and side).
Cross-peaks indicate the presence of exchange.
ppm
1.2
1.4
1.6
1.7 1.6 1.5 1.4 1.3 1.2 1.1













2 – 1H (ppm)
1.8
ppm 
iv
Figure S4:
Low-temperature 1H NMR spectra acquired at 400 MHz.
Temperature/K
220
230
240
250
260
270
280
290
300
1.5
Temperature/K




220


230



240



250



260



270



280



290



300

1.0 
0.5
0.0

2 –1H (ppm)
 10
ppm-1.0
-1.5
-2.0
v
ppm