Angewandte
Chemie
unsaturated substrate, n-pentane (30 mL), and H2 (30 bar). The
ensemble was heated to the appropriate temperature and then stirred
(1500 rpm) for the desired time, after which the vessel was cooled to
ambient temperature and depressurised. The liquid contents were
analysed by GC and GC–MS. Above 1500 rpm, the rates were
independent of the agitation speed at all the temperatures studied,
thus indicating the absence of mass transfer resistance.
Received: December 2, 2002
Revised: March 13, 2003 [Z50667]
Keywords: arenes · heterogeneous catalysis · hydrogenation ·
.
palladium· rhodium
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[6] NMR Data ([D7]DMF, 208C,
J
in Hz): 31P{1H} NMR
(81.01 MHz): d = 11.0 ppm (d, 1J(P,Rh) = 122.6); 1H NMR
(200.13 MHz): d = 7.88 (d, 3J(H,H) = 8.1, 2H; m-H-SO3C6H4),
7.71 (d, 3J(H,H) = 8.1, 2H; o-H-SO3C6H4), 7.30 (m, 6H; p-H-
PPh2), 7.2–7.1 (m, 24H; o- and m-H-PPh2), 6.61 (m, 2H; CH-
C6H8), 3.52 (s, 2H; CH2C), 3.45 (m, 2H; CH-C6H8), 2.91 (br s, 6H;
CH2P), 1.35 (m, 2H; Hb(CH2)-C6H8), 1.23 ppm (m, 2H;
Ha(CH2)-C6H8).
[7] Crystal data: yellow crystals (0.3 0.25 0.25 mm), monoclinic,
space group P21/n, a = 13.513(5), b = 18.308(5), c = 19.539(5) ,
b = 94.350(5)8, V= 4820(3) 3, Z = 4, 1calcd = 1.415 gcmÀ3, m =
0.546 mmÀ1, MoKa (l = 0.71609 ), T= 293(2) K, 6674 independ-
ent reflections. Refinement on all data converged at R1 = 0.0678,
wR2 = 0.1113, GOF = 0.9912. CCDC-198527 contains the supple-
mentary crystallographic data for this paper. These data can be
html (or from the Cambridge Crystallographic Data Centre, 12
Union Road, Cambridge CB21EZ, UK; fax: (+ 44)1223-336-033;
or deposit@ccdc.cam.ac.uk).
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Angew. Chem. Int. Ed. 2003, 42, 2636 – 2639
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