RESEARCH FRONT
588
B. Saha et al.
(40 mg, 0.05 mmol) and the solution was stirred for 8 h at room
temperature. The red solution was concentrated under reduced
pressure and hexane was added to induce precipitation. Red
precipitate was washed with hexane and dried under vacuum.
Crystals suitable for X-ray diffraction were grown by layering
hexane over a concentrated dichloromethane solution of 1 inside
an 8 mm o.d. vacuum-sealed glass tube (44 mg, 82%). dH
(500 MHz, CDCl3, 294 K) 9.71 (d, J 5.5 Hz, 1H, NP), 9.26 (d, J
5.2 Hz, 1H, NP), 8.56 (d, J 8.55 Hz, 1H, NP), 7.96 (q, J 3.05 Hz,
1H, NP), 7.67 (d, J 8.25 Hz, 1H, NP), 7.35 (s, 2H, Mesityl), 2.00
(s, 3H, Methylmesityl), 1.96 (s, 6H, Methylmesityl), 1.72 (s, 3H,
Methylacetate). n(KBr)/cmꢀ1 (BF4ꢀ) 1055; n(KBr)/cmꢀ1 (OAc)
1432. Anal. Calcd for C38H38N4O4B2F8Rh2: C 45.91, H 3.85,
N 5.64. Found: C 45.86, H 3.78, N 5.57%.
fellowship. B.S., A.S. thank CSIR and W.R. thanks UGC, India for
fellowships.
References
[1] J. K. Bera, N. Sadhukhan, M. Majumdar, Eur. J. Inorg. Chem. 2009,
4023 and references therein. doi:10.1002/EJIC.200900312
[2] M. Majumdar, A. Sinha, T. Ghatak, S. K. Patra, N. Sadhukhan,
S. M. W. Rahaman, J. K. Bera, Chem. Eur. J. 2010, 16, 2574.
doi:10.1002/CHEM.200902797
[3] R. K. Das, B. Saha, S. M. W. Rahaman, J. K. Bera, Chem. Eur. J. 2010,
16, 14459. doi:10.1002/CHEM.201001960
[4] A. Sinha, T. Ghatak, J. K. Bera, Dalton Trans. 2010, 39, 11301.
doi:10.1039/C0DT00679C
[5] S. K. Patra, S. M. W. Rahaman, M. Majumdar, A. Sinha, J. K. Bera,
Chem. Commun. 2008, 2511. doi:10.1039/B803632B
[6] N. Sadhukhan, J. K. Bera, Inorg. Chem. 2009, 48, 978. doi:10.1021/
IC801586D
[7] S. K. Patra, J. K. Bera, Organometallics 2007, 26, 2598. doi:10.1021/
OM070139J
Synthesis of [Ru(Mes-NP)2(CH3CN)2](BF4)2 (2)
The Mes-NP (27 mg, 0.1 mmol) and [n-Bu4N][BF4] (16 mg,
0.05 mmol) were added to a dichloromethane solution of cis-
[Ru2(CO)4(CH3CN)6](BF4)2 (40 mg, 0.05 mmol) and the solu-
tion was stirred for 24 h at room temperature. The red solution
was concentrated under reduced pressure and hexane was added
to induce precipitation. The red precipitate was washed with
hexane and dried under vacuum. Crystals suitable for X-ray
diffraction were grown by layering hexane over a concentrated
dichloromethane solution of 2 inside an 8 mm o.d. vacuum-
sealed glass tube (37 mg, 80%). dH (500 MHz, CD3CN, 294 K)
9.45 (d, J 9.5 Hz, 1H, NP), 8.50 (d, J 4.25 Hz, 1H, NP), 8.47
(d, J 5.2 Hz, 1H, NP), 7.68 (q, J 3.2 Hz, 1H, NP), 7.14 (s, 2H,
Mesityl), 2.49 (s, 3H, Methylmesityl), 2.33 (s, 6H, Methyl).
n(KBr)/cm–1 (BF4ꢀ) 1055. Anal. Calcd for C38H38N6B2F8Ru:
C 53.48, H 4.49, N 9.85. Found: C 53.42, H 4.41, N 9.79%.
[8] S. K. Patra, N. Sadhukhan, J. K. Bera, Inorg. Chem. 2006, 45, 4007.
doi:10.1021/IC0600073
[9] M. Majumdar, S. K. Patra, M. Kannan, K. R. Dunbar, J. K. Bera, Inorg.
Chem. 2008, 47, 2212. doi:10.1021/IC702298V
[10] M. Majumdar, S. M. W. Rahaman, A. Sinha, J. K. Bera, Inorg. Chim.
Acta 2010, 363, 3078. doi:10.1016/J.ICA.2010.03.044
[11] S. K. Patra, J. K. Bera, Organometallics 2006, 25, 6054. doi:10.1021/
OM060774þ
[12] S. K. Patra, M. Majumdar, J. K. Bera, J. Organomet. Chem. 2006, 691,
4779. doi:10.1016/J.JORGANCHEM.2006.07.033
[13] M. A. Petrukhina, A. S. Filatov, Y. Sevryugina, K. W. Andreini,
S. Takamizawa, Organometallics 2006, 25, 2135. doi:10.1021/
OM051100M
[14] M. A. Petrukhina, Y. Sevryugina, A. Yu. Rogachev, E. A. Jackson,
L. T. Scott, Angew. Chem. Int. Ed. 2006, 45, 7208. doi:10.1002/ANIE.
200602568
[15] M. A. Petrukhina, Angew. Chem. Int. Ed. 2008, 47, 1550. doi:10.1002/
ANIE.200704783
X-Ray Data Collection and Refinement
˚
[16] A shorter Rh–Rh distance of 2.356(1) A is found in cis-[Rh2(m-
Single-crystal X-ray studies were performed on a CCD Bruker
SMART APEX diffractometer equipped with an Oxford
Instruments low-temperature attachment. All data were col-
lected at 100(2) K using graphite monochromated MoKa radia-
.
O2CCH3)2(Z3-pynp)(Z1-pynp)(NCCH3)2](BF4)(PF6) 2CH3CN
compound. However the less yield of this compound regarded as
minor product of the reaction. C. S. Campos-Ferna´ndez, L. M.
Thomson, J. R. Gala´n-Mascaro´s, X. Ouyang, K. R. Dunbar, Inorg.
Chem. 2002, 41, 1523. doi:10.1021/IC010996U
˚
tion (la 0.71073 A). The frames were indexed, integrated, and
scaled using the SMART and SAINT software packages,[61] and
the data were corrected for absorption using the SADABS pro-
grams.[62] Structures were solved and refined with the SHELX
suite of programs[63] as implemented in X-Seed.[64] The figures
were drawn using ORTEP.[65] All the hydrogen atoms were
included at geometrically calculated positions in the final stages
of the refinement and were refined according to the ‘riding
model’. All non-hydrogen atoms were refined with anisotropic
thermal parameters unless mentioned otherwise. Pertinent
crystallographic data for compounds 1 and 2 are summarized in
Table 4. CCDC 810328 (1) and 810329 (2) contain the supple-
mentary crystallographic data for this paper. These data can be
obtained free of charge from the Cambridge Crystallographic
[17] I. B. Baranovskii, M. A. Golubnichaya, L. M. Dikareva, Russ. J. Inorg.
Chem. 1982, 27, 1158.
[18] L. M. Dikareva, M. A. Golubnichaya, I. B. Baranovskii, Russ. J. Inorg.
Chem. 1988, 33, 1179.
[19] F. P. Pruchnik, A. Jutarska, Z. Ciunik, M. Pruchnik, Inorg. Chim. Acta
2004, 357, 3019. doi:10.1016/J.ICA.2004.02.017
[20] T. Yoshimura, K. Umakoshi, Y. Sakai, Chem. Lett. 1999, 28, 267.
doi:10.1246/CL.1999.267
[21] A. P. Kochetkova, L. B. Sveshnikova, V. M. Stepanovich, V. I. Sokol,
Sov. J. Coord. Chem. 1982, 8, 281.
[22] V. I. Sokol, M. A. Porai-Koshits, A. P. Kochetkova, L. B. Sveshnikova,
Sov. J. Coord. Chem. 1984, 10, 461.
[23] E. Galdecka, Z. Galdecki, F. P. Pruchnik, P. Jakimowciz, Trans. Met.
Chem. 2000, 25, 315. doi:10.1023/A:1007053619224
[24] C. A. Crawford, J. H. Matonic, J. C. Huffman, K. Folting, K. R. Dunbar,
G. Christou, Inorg. Chem. 1997, 36, 2361. doi:10.1021/IC9610288
[25] C. A. Crawford, J. H. Matonic, W. E. Streib, J. C. Huffman, K. R.
Dunbar, G. Christou, Inorg. Chem. 1993, 32, 3125. doi:10.1021/
IC00066A026
[26] M. Calligaris, L. Campana, G. Mestroni, M. Tornatore, E. Alessio,
Inorg. Chim. Acta 1987, 127, 103. doi:10.1016/S0020-1693(00)
88369-3
Accessory Publication
The accessory publication contains mechanism of alcohol oxi-
dation to aldehyde, general procedures for the catalysis reac-
tions and relevant metrical parameters for compounds 1 and 2.
[27] T. Glowaik, H. Pasternak, Acta Crystallogr. 1987, C43, 1036.
[28] T. Glowaik, F. Pruchnik, M. Zuber, Pol. J. Chem. 1991, 65, 1749.
[29] M. A. M. Daniels, N. Mehmet, D. A. Tocher, J. Chem. Soc., Dalton
Trans. 1986, 1257.
Acknowledgements
This work is financially supported by the Department of Science
and Technology (DST), India. J.K.B. thanks DST for the Swarnajayanti