sure yielding the corresponding compounds containing pen-
dant dpquin ligands. Yields: R = H, 10; Me, 15; Et, 5% (Found:
C, 49.9; H, 2.8; N, 2.5. Calc. for C47H33F6N2O6P3Ru2: C, 49.9;
H, 2.9; N, 2.5. Found: C, 50.5; H, 3.6; N, 2.5. Calc. for
C48H35F6N2O6P3Ru2: C, 50.4; H, 3.1; N, 2.5. Found: C, 50.5; H,
3.3; N, 2.6. Calc. for C49H37F6N2O6P3Ru2: C, 50.8; H, 3.2; N,
2.4%).
References
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11 K.-B. Shiu, W.-N. Guo, T.-J. Chan, J.-C. Wang, L.-S. Liou,
S.-M. Peng and M.-C. Cheng, Organometallics, 1995, 14, 1732.
12 A. P. Steyn, unpublished work.
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Chem., 1972, 40, C67.
14 M. Rotem, Y. Shvo, I. Goldberg and U. Shmueli, Organometallics,
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Chem., 1986, 314, 185.
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20 S. J. Sherlock, M. Cowie, E. Singleton and M. M. de V. Steyn,
J. Organomet. Chem., 1989, 361, 353.
21 J. S. Field, R. J. Haines, J. Sundermeyer and S. F. Woollam, J. Chem.
Soc., Dalton Trans., 1993, 2735.
22 J. S. Field, R. J. Haines, J. Sundermeyer, A. Wood and
S. F. Woollam, Polyhedron, 1994, 12, 2425.
23 G. Newkome and D. Hager, J. Org. Chem., 1978, 43, 947.
24 W. K. Schauerte, M.Sc. Thesis, University of Natal, Pietermaritz-
burg, 1992.
25 J. S. Field, R. J. Haines, C. J. Parry and S. H. Sookraj, S. Afr. J.
Chem., 1993, 46, 70.
[Ru2{ì-ç2-OC(R)O}(CO)2(ì-dpbipy)2]PF6 (R ؍
H, Me or
Et). A suspension of the appropriate carboxylate-bridged
polymer [{Ru2[µ-η2-OC(R)O]2(CO)4}n] (0.3 mmol) and dpbipy
(0.205 g, 0.6 mmol) in n-butanol (10 cm3) was refluxed at 120 ЊC
for 24 h. The solution slowly changed from orange-yellow
through to dark brown. The reaction solution was cooled to
room temperature and filtered. A hot solution of NH4PF6
(0.105 g, 0.65 mmol) in butan-1-ol was added dropwise with
stirring to precipitate the product as a brown powder. This was
filtered off, washed with diethyl ether (5 × 5 cm3) and dried in
vacuo for 12 h at 40 ЊC effectively to remove any residual
n-butanol. Recrystallisation of the product from acetonitrile–
diethyl ether (1:1 v/v) at Ϫ25 ЊC afforded the analytically pure
product as dark brown needles. Yields: R = H, 70; Me, 80; Et,
65% (Found: C, 49.9; H, 3.0; N, 4.7. Calc. for C47H35F6N4-
O4P3Ru2: C, 50.0; H, 3.1; N, 5.0. Found: C, 50.0; H, 3.7; N, 4.7.
Calc. for C48H37F6N4O4P3Ru2: C, 50.4; H, 3.3; N, 4.9. Found: C,
50.4; H, 3.1; N, 4.7. Calc. for C49H39F6N4O4P3Ru2: C, 50.9; H,
3.4; N, 4.8%).
Crystallography
Crystal data for [Ru2{µ-η2-OC(Me)O}2(CO)4(dppy)2], [Ru2-
{µ-η2-OC(H)O}(CO)4(µ-dppy)2]PF6,
and
[Ru2{µ-η2-OC-
(Me)O}(CO)2(µ-dpbipy)2]PF6 as well as details of the structure
solution and refinement are summarised in Table 5.
Intensity data were collected at 295 K on a CAD4 diffract-
ometer by the variable-speed ω–2θ scan method in the range
3 р 2θ р 46Њ with Mo-Kα radiation (λ = 0.710 69 Å) the data
being corrected for absorption by the ψ-scan method.26 The
structures were solved by standard Patterson methods and sub-
sequently completed by Fourier recycling and full-matrix least-
squares refinement based on F.27 Non-hydrogen atoms were
assigned anisotropic thermal factors and the hydrogen atoms a
single common thermal factor; the latter were placed in calcu-
lated positions. Neutral atom scattering factors were used with
corrections for anomalous dispersion.28
26 A. C. T. North, D. C. Philips and F. A. Mathews, Acta Crystallogr.,
Sect. A, 1968, 24, 35.
27 G. M. Sheldrick, SHELX 76, Program for Crystal Structure Solu-
tion and Refinement, University of Cambridge, 1976.
28 International Tables for X-Ray Crystallography, Kynoch Press,
Birmingham, 1974, vol. 4, pp. 99, 148.
CCDC reference number 186/571.
Acknowledgements
The authors express their sincere gratitude to the Foundation
for Research Development and the University of Natal for
financial support.
Received 18th March 1997; Paper 7/01897E
2848
J. Chem. Soc., Dalton Trans., 1997, Pages 2843–2848
Field, John S.
