by allowing diethyl ether to diffuse into a concentrated CH2Cl2
solution at −10 ◦C. Red crystals of [(o-O2C6Cl4)(Ph3P)(OC)2Ru(l-
CN)Ru(CO)2(PPh3)(o-O2C6Cl4)]·CH2Cl2 8·CH2Cl2 and [(o-
O2C6Cl4)(Ph3P)(OC)2Ru(l-CN)Ru(CO)2{P(OPh)3}(o-O2C6Cl4)]·
2CH2Cl2 9A·2CH2Cl2 were grown by allowing diethyl ether to
diffuse into a concentrated CH2Cl2 solution, of 8 and 9 res-
pectively, at −10 ◦C.
315; G. A. Carriedo, N. G. Connelly, S. Alvarez, E. Perez-Carreno and
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8 C. G. Pierpont and H. H. Downs, Inorg. Chem., 1975, 14, 343.
9 M. J. Freeman, PhD Thesis, University of Bristol, 1984.
10 A. P. Meacham, K. L. Druce, Z. R. Bell, M. D. Ward, J. B. Keister and
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Many of the details of the structure analyses of [{Ru(CO)2-
{P(OPh)3}(l-o-O2C6Cl4)}2], [NEt4]+1−·0.5CH2Cl2, [NEt4]+8−·
0.5CH2Cl2, 8·CH2Cl2 and 9A·2CH2Cl2 are listed in Table 10.
The orientation of the cyanide bridges in complexes 8 and 8−
was assigned on the basis of the best agreement for the thermal
parameters and occupancy factors for the C and N atoms, after
refinement in two alternative models in which the C and N atoms
were exchanged. This led to a 50 : 50 ratio of CN to NC in 8−, and
a 65(7) : 35(7) ratio in 8. The structure of [NEt4]+1−·0.5CH2Cl2
contains two 1− anions, two [NEt4]+ cations (one of which is
disordered over two positions) and one disordered molecule of
CH2Cl2 in the asymmetric unit. The CH2Cl2 molecule in the
structure of [NEt4]+8−·0.5CH2Cl2 is also disordered over two
positions.
CCDC reference numbers 633571–633575.
For crystallographic data in CIF or other electronic format see
DOI: 10.1039/b700648a
Acknowledgements
12 L. Pasimeni, M. Brustolon and C. Corvaja, J. Magn. Reson., 1976, 21,
259.
We thank UUK for an ORS Postgraduate Scholarship (to S.O.),
the Royal Thai Government for a Postgraduate Scholarship (to
A.K.) and Dr S. Vickers and Prof. M.D. Ward of the University
of Sheffield for the IR spectroelectrochemical study of the
oxidation of [NEt4][(o-O2C6Cl4)(Ph3P)(OC)2Ru(l-CN)Ru(CO)2-
{P(OPh)3}(o-O2C6Cl4)] [NEt4]+9−.
13 D. A. Dows, A. Haim and W. K. Walmarth, J. Inorg. Nucl. Chem., 1961,
21, 33.
14 S. Bhattacharya and C. G. Pierpont, Inorg. Chem., 1994, 33, 6038.
15 S. Bhattacharya and C. G. Pierpont, Inorg. Chem., 1991, 30, 1511.
16 T. Wada, T. Fujihara, M. Tomori, D. Ooyama and K. Tanaka, Bull.
Chem. Soc. Jpn., 2004, 77, 741.
17 S. R. Boone, G. H. Purser, H.-R. Chang, M. D. Lowery, D. N.
Hendrickson and C. G. Pierpont, J. Am. Chem. Soc., 1989, 111,
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18 N. G. Connelly, D. J. H. Emslie, O. D. Hayward, A. G. Orpen and M. J.
Quayle, J. Chem. Soc., Dalton Trans., 2001, 875.
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20 N. G. Connelly and W. E. Geiger, Chem. Rev., 1996, 96, 877.
References
1 See, for example, G. A. Carriedo, N. G. Connelly, M. C. Crespo, I. C.
Quarmby, V. Riera and G. H. Worth, J. Chem. Soc., Dalton Trans., 1991,
2294 | Dalton Trans., 2007, 2283–2294
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