1.32 mmol) in THF (3 mL). The mixture was left at [35 ¡C
for 5 h. Addition of 12 mL of cold ([35 ¡C) hexane precipi-
tated a white solid. It was isolated by Ðltration, washed with
3 ] 3 mL of hexane and dried under vacuum. Yield: 684 mg
Found: C, 47.89; H, 7.85; N, 1.54. IR (Nujol): m
1790, m
ReH
ReH
or/and m
1597, m 1500 cm~1. 1H NMR (200 MHz, THF-
C/C
NO
d ): d [5.45 (td, 2J \ 22.1 Hz, 2J
\ 8.3, 1H, ReH),
8
HhP
HhH
[3.78 (td, 2J \ 31.4 Hz, 1H, ReH), 1.15, 1.19 (dvt, vJ
HhP
\
HhP
(60%). IR (Nujol): m
2058, m and m
1852, m
or/and
6.3 Hz, 3J
\ 5.3 Hz, 36H, CH ), 2.36 (m, 6H, CH), 3.57 (s,
C. C
CO
RhH
RuH
HhH
3
m
1597 cm~1. 5: 1H NMR (200 MHz, THF-d ): d [11.10
24H, crown-CH ), 4.81, 5.83 (d, 2J
\ 7.1 Hz, 2H, xCH )
C/C
8
2
HhH
2
(td, 2J \ 22.3 Hz, 2J
\ 7.0, 1H, RuH), [8.27 (td,
6.60, 6.86, 7.40 (m, 5H, C H ). 31PM1HN NMR (80 MHz, THF-
HhP
HhH
6 5
2J \ 26.1 Hz, 1H, RuH), 1.30 (dvt, vJ \ 6.3 Hz,
d ): d 42.7. 13CM1HN NMR (50 MHz, THF-d ): d 20.78, 21.64
HhP
HhH
HhP
8
8
3J
\ 6.0 Hz, 36H, CH ), 2.21 (m, 6H, CH), 3.55 (s, 24H,
(s, CH ), 29.51 (vt, vJ \ 10.1 Hz, PCH), 71.12 (s, crown-
ChP
CH ), 120.30 (s, xCH ), 121.18, 126.07, 128.96 (s, CH, Ph),
3
3
crown-CH ), 6.5È7.4 (m, 5H, C H ). 31PM1HN NMR (80 MHz,
2
6
5
2
2
THF-d ): d 84.0. 13CM1HN NMR (50 MHz, THF-d ): d 21.45,
165.75 (s, C , Ph), 182.06 (t, 2J \ 5.0 Hz, RewCPh).
ipso ChP
8
8
21.61 (s, CH ), 28.79 (vt, vJ \ 9.1 Hz, PCH), 71.12 (s,
Assignment of the 13C signals is conÐrmed by a gated-
3
ChP
crown-CH ), 113.24 (s, y CPh), 119.84, 127.64, 130.86 (s, CH,
decoupled 13C experiment: d 120.30 (dd, 1J
\ 142, 145 Hz,
2
ChH
Ph), 135.30 (s,
C
,
Ph), 148.24 (t, 2J \ 13.3 Hz,
xCH ).
ipso
ChP
2
RuwCy ), 212.35 (t, 2J \ 9.5 Hz, RuwCO). 6: 1H NMR
ChP
(200 MHz, THF-d ): d [12.39 (td, 2J \ 25.7 Hz, 2J
\
8
HhP
HhH
Acknowledgements
7.0, 1H, RuH), [7.52 (td, 2J \ 27.8 Hz, 1H, RuH), 1.17
HhP
(dvt, vJ \ 6.3 Hz, 3J
HhP
\ 6.0 Hz, 36H, CH ), 2.12 (m, 6H,
HhH
3
Wilfrid Laurier University supported this research in the form
of a start-up grant to D.G.G. We thank the Natural Sciences
and Engineering Research Council (NSERC) of Canada for
the undergraduate student research award to B.R. The com-
petent technical assistance of Ms. Margaret Szymanska is
gratefully acknowledged.
CH), 3.55 (s, 24H, crown-CH ), 5.20, 5.55 (d, 2J
\ 7.6 Hz,
2
HhH
2H, xCH ) 6.5È7.4 (m, 5H, C H ). 31PM1HN NMR (80 MHz,
2
6 5
THF-d ): d 81.2. 13CM1HN NMR (50 MHz, THF-d ): d 21.05,
8
8
21.97 (s, CH ), 28.92 (vt, vJ \ 8.4 Hz, PCH), 71.12 (s,
ChP
crown-CH ), 121.62 (t, 3J \ 2.1 Hz, xCH ), 120.40, 125.79,
ChP
3
2
2
128.93 (s, CH, Ph), 167.82 (s, C , Ph), 191.96 (t, 2J \ 9.3
ipso
ChP
Hz, RuwCPh), 212.59 (t, 2J \ 10.5 Hz, RuwCO). Assign-
ChP
ment of the 13C signals is conÐrmed by an APT (attached
References
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3 2
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2
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3 2
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Ðltration, washed with 2 ] 5 mL of hexane and dried under
vacuum. Yield: 500 mg (75%). Anal. calcd for
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7 2
New J. Chem., 1999, 1È3
3