A. Sua´rez et al. / Journal of Organometallic Chemistry 656 (2002) 270Á
/
273
273
1
O): 2061s, 1976s, 1962s, 1920s. H-NMR: 3.50 (s,
n(CÄ
/
A
ꢁ3. Complex scattering factors were taken from the
program package SHELXL93 [19].
3H, NMe). M.p.: 179 8C.
3.2.3. [Mn{2-(CMeÄ
CHN(Me)}(CO)4] (3), [Mn{2-(CPhÄ
NCHÄCHN(Me)}(CO)4] (4)
/
CPh)C6H4CÄ
/
NCHÄ
/
/
CMe)C6H4CÄ
/
4. Supporting information available
/
A reaction time of 8 h was used. The final residue gave
a mixture of 3 and 4 in a 1:1 molar ratio as calculated
from the integrals in the 1H-NMR spectra. Both
compounds could be obtained from the mixture in
pure form by fractional recrystallization. The mixture
was dissolved in chloroform (ca. 15 cm3), filtered, n-
hexane carefully added and the resultant solution kept
Crystallographic data for structural analysis have
been deposited with the Cambridge Crystallographic
Data Centre, CCDC no. 177060 for compound 5.
Copies of the information may be obtained free of
charge from The Director, CCDC, 12 Union Road,
Cambridge CB2 1EZ, UK (Fax: ꢀ44-1223-336033; e-
/
mail: deposit@ccdc.cam.ac.uk
at ꢁ
/
15 8C for 24 h. Yellow crystals of 3 were formed.
The chloroformÁ/n-hexane solution was evaporated to
dryness giving 4 as a yellow solid. Overall yield: 74%. 3:
Anal. Found: C, 62.4; H, 3.6; N, 6.5. C22H17N2O4Mn
Acknowledgements
requires: C, 62.7; H, 3.8; N, 6.3%. IR: n(CÄ
/
O): 2060s,
1
1990s, 1968s, 1921s. H-NMR: 3.37 (s, 3H, NMe), 1.81
(s, 3H, CMe). M.p.: 172 8C. 4: Anal. Found: C, 62.3; H,
3.6; N, 6.6. C22H17N2O4Mn requires: C, 62.7; H, 3.8; N,
We thank the Universidad de A Coruna for financial
˜
support.
6.3%. IR: n(CÄ
/
O): 2060s, 1985s, 1965s, 1928s. 1H-
NMR: 3.68 (s, 3H, NMe), 1.96 (s, 3H, CMe). M.p.:
176 8C.
References
3.2.4. [Mn{2-(CMeÄ
CHN(Me)C(Ph)}(CO)4] (5), [Mn{2-(CPhÄ
CHN(Me)C(Ph)}(CO)4] (6)
/
CPh)C6H4CNÄ
/
[1] A.D. Ryabov, Synthesis 3 (1985) 233.
/
[2] M. Pfeffer, Recl. Trav. Chim. Pays-Bas 109 (1990) 567.
[3] J. Spencer, M. Pfeffer, Adv. Met. Org. Chem. 6 (1998) 103.
[4] L. Main, B.K. Nicholson, Adv. Met. Org. Chem. 3 (1994) 1.
[5] R.C. Cambie, P.S. Rutledge, D.R. Welch, P.D. Woodgate, J.
Organomet. Chem. 467 (1994) 237.
CMe)C6H4CNÄ
/
Overall yield: 82%. 5: Anal. Found: C, 67.1; H, 3.8; N,
5.5. C28H21N2O4Mn requires: C, 67.4; H, 4.1; N, 5.4%.
1
O): 2079s, 1984s, 1972s, 1930s. H-NMR: 3.67
IR: n(CÄ
/
[6] W. Tully, L. Main, B.K. Nicholson, J. Organomet. Chem. 507
(1996) 103.
(s, 3H, NMe), 1.61 (s, 3H, CMe). M.p.: 176 8C. 6: Anal.
Found: C, 67.2; H, 4.0; N, 5.3. C28H21N2O4Mn requires:
[7] P. De Shong, D.R. Sidler, P.J. Rybczynski, G.A. Slough, A.L.
Rheingold, J. Am. Chem. Soc. 110 (1988) 2575.
[8] W.J. Grigsby, L. Main, B.K. Nicholson, Organometallics 12
(1993) 397 (see reference [6]).
C, 67.4; H, 4.1; N, 5.4%. IR: n(CÄ
/
O): 2065s, 1980s,
1965s, 1935s. H-NMR: 3.62 (s, 3H, NMe), 1.87 (s, 3H,
1
CMe). M.p.: 179 8C.
[9] G.J. Depree, L. Main, B.K. Nicholson, J. Organomet. Chem. 551
(1998) 281.
[10] W. Tully, L. Main, B.K. Nicholson, J. Organomet. Chem. 633
(2001) 162.
3.3. X-ray structure determination
[11] M. Pfeffer, E.P. Urriolabeitia, J. Fischer, Inorg. Chem. 34 (1995)
643.
For complex 5 three-dimensional, r.t. X-ray data were
collected in the range 3.5B
/
2u B45.08 on a Siemens P4
/
[12] A. Sua´rez, J.M. Vila, M.T. Pereira, E. Gayoso, M. Gayoso, J.
Organomet. Chem. 335 (1987) 359.
diffractometer by the omega scan method. 4392 reflec-
tions were measured, all of which were corrected for
Lorentz and polarisation effects. The structure was
solved by direct methods and refined by full-matrix
least-squares on F2. Hydrogen atoms were included in
calculated positions and refined in riding mode. Refine-
[13] K. Nakamoto, Infrared and Raman Spectra of Inorganic and
Coordination Compounds, 5th ed., Wiley, New York, 1997.
[14] J. Spencer, M. Pfeffer, N. Kyritsakas, J. Fischer, Organometallics
14 (1995) 2214.
[15] R.G. Little, R.J. Doedens, Inorg. Chem. 12 (1973) 844 (and
references therein).
[16] J.M. Cooney, L.H.P. Gommans, L. Main, B.K. Nicholson, J.
Organomet. Chem. 349 (1988) 197.
ment converged at a final Rꢂ
/
0.0419 (wR2ꢂ0.1148 for
/
all 3331 unique data, 325 parameters, mean and max-
imum d/s 0.000, 0.001), with allowance for the thermal
anisotropy of all non-hydrogen atoms. Minimum and
[17] W.L.F. Armarego, D.D. Perrin, Purification of Laboratory
Chemicals, 4th ed., Butterworth-Heinemann, Oxford, 1997.
[18] M.I. Bruce, M.J. Liddell, G.N. Pain, Inorg. Synth. 26 (1989) 171.
maximum final electron density ꢁ
/
0.238 and 1.203 e
[19] G.M. Sheldrick, University of Gottingen, Germany, 1993.
¨