1612
R.J. Abernethy et al. / Inorganica Chimica Acta 358 (2005) 1605–1613
(d) R. Garcia, A. Domingos, A. Paulo, I. Santos, R. Alberto,
Inorg. Chem. 41 (2002) 2422.
pound was characterized by comparison of spectro-
scopic data with those previously reported [10].
[4] (a) H.M. Alvarez, T.B. Tran, M.A. Richter, D.M. Alyounes, D.
Rabinovich, J.M. Tanski, M. Krawiec, Inorg. Chem. 42 (2003)
2149;
4.6. Synthesis of [W(CO){H2B(mt)2}2]
(b) H.M. Alvarez, M. Krawiec, B.T. Donovan-Merkert, M.
Fouzi, D. Rabinovich, Inorg. Chem. 40 (2001) 5736;
(c) H.M. Alvarez, J.M. Tanski, D. Rabinovich, Polyhedron 23
(2004) 395.
A mixture of [W(„CC6H2Me3-2,4, 6)Cl(CO)2(py)2]
(2.00 g, 3.51 mmol) and Na[H2B(mt)2] (1.86 g, 7.02
mmol) in tetrahydrofuran (150 ml) was heated under re-
flux for 24 h. The mixture was allowed to cool to room
temperature over several hours, during which copious
amounts of a brilliant green solid precipitated from
the reaction mixture. The solid was filtered off and
washed with dichloromethane (3 · 30 ml) and water
(2 · 20 ml) to remove residual NaCl formed in the reac-
tion. The solid was then washed with warm ethanol, and
dried in vacuo, to yield the desired product as a dark
green powder. Yield = 0.93 g (39%). IR Nujol: 2446,
2441 [m(B-H)], 2246 [m(BHMo)], 1765 [m(CO)]; 1555,
1191, 1170 cmꢀ1. IR Solution: m(CO) = 1785 (CH2Cl2),
[5] M.R.St.-J. Foreman, A.F. Hill, N. Tshabang, A.J.P. White, D.J.
Williams, Organometallics 22 (2003) 5593.
[6] M.R.St.-J. Foreman, A.F. Hill, G.R. Owen, A.J.P. White, D.J.
Williams, Organometallics 22 (2003) 4446.
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Chem., Int. Ed. Engl. 38 (1999) 2759.
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Szameitat, Angew. Chem., Int. Ed. Engl. 28 (1989) 210.
[9] A.F. Hill, J.M. Malget, A.J.P. White, D.J. Williams, Eur. J.
Inorg. Chem. (2004) 818.
[10] E. Bannwart, H. Jacobsen, F. Furno, H. Berke, Organometallics
19 (2000) 3605.
[11] (a) G.A. McDermott, A.M. Dorries, A. Mayr, Organometallics 6
(1987) 925;
1
1764 (THF); 1771 (dmso) cmꢀ1. NMR H (300 MHz,
(b) A. Mayr, G.A. McDermott, A.M. Dorries, Organometallics 4
(1985) 608.
d6-dmso, 25 ꢁC): d = ꢀ3.58 (s.v.br, 1 H, B–H–W), 0.03
[12] R.J. Abernethy, A.F. Hill, A.C. Willis, in preparation.
[13] M.R.St.-J. Foreman, A.F. Hill, A.J.P. White, D.J. Williams,
Organometallics 22 (2003) 3831.
(s.v.br. 1 H, BH), 2.90, 3.45 (s · 2, 6 H · 2, NCH3),
3
6.83, 7.27 [d · 2, 2 H · 2, J(HH) = 1.5, C3H2N2], 6.94,
3
7.31 [d · 2, 2 H · 2, J(HH) = 2.0 Hz, CH=CH] ppm.
[14] M. Shimoi, S.-I. Nagai, M. Ichikawa, Y. Kawano, K. Katoh, M.
Uruichi, H. Ogino, J. Am. Chem. Soc. 121 (1999) 11704.
[15] L. Ricard, R. Weiss, W.E. Newton, G.J.-J. Chen, J.W. McDon-
ald, J. Am. Chem. Soc. 100 (1978) 1318.
11B{1H} (96.2 MHz, d6-dmso, 25 ꢁC): d = ꢀ4.97 Anal.
calc. for C17H24B2N4OS4W.2CH2Cl2: C, 26.54; H,
3.28; N, 13.03. Found C, 26.6; H, 3.2; N, 13.4%.
APCI-MS: m/z(%) [assignment] 691(40) [M]+, 662(70)
[M ꢀ CO)]+. Crystal data: C17H24B2N8OS4W Æ CH2Cl2;
[16] M.A. Bennett, I.A. Boyd, G.B. Robertson, W.A. Wickramasin-
ghe, J. Organomet. Chem. 290 (1985) 181.
[17] J.L. Templeton, R.S. Herrick, C.A. Rusik, C.E. McKenna, J.W.
McDonald, W.E. Newton, Inorg. Chem. 24 (1985) 1383.
[18] K.-M. Sung, R.H. Holm, Inorg. Chem. 39 (2000) 1275.
[19] (a) Recent examples of pyrazolyl borate cleavage include: T.R.
Mr = 775.10;
monoclinic;
P21/n;
˚
a = 9.5897(1);
b = 19.1292(2); c = 15.0943(2) A; b = 91.5100 (5)ꢁ;
V = 2767.99(5) A ; Z = 4; Dx = 1.860 g cmꢀ3; l(Mo
3
˚
´
´
Belderraın, M. Paneque, E. Carmona, E. Gutierrez-Puebla, M.A.
Monge, C. Ruiz-Valero, Inorg. Chem. 41 (2002) 425;
(b) L.M.L. Chia, S. Radojevic, I.J. Scowen, M. McPartlin, M.
Halcrow, J. Chem. Soc., Dalton Trans. (2000) 133;
(c) G. Bellachioma, G. Cardaci, V. Gramlich, A. Macchioni,
F. Pieroni, L.M. Venanzi, J. Chem. Soc., Dalton Trans.
(1998) 947;
Ka) = 46.98 cmꢀ1; T = 200 K, green plate; 64499 mea-
sured reflections (2h < 55ꢁ), F refinement, R = 0.023,
wR = 0.016 for 4431 independent absorption corrected
reflections [I > 3r(I)], 337 parameters, CCDC 235063.
(d) A. Albinati, M. Bovens, H. Rueger, L.M. Venanzi, Inorg.
¨
Chem. 36 (1997) 5991.
Acknowledgement
[20] (a) S. Trofimenko, Inorg. Chem. 9 (1970) 2493;
(b) S. Trofimenko, J. Am. Chem. Soc. 91 (1969) 3183.
[21] C.A. Kosky, P. Ganis, G. Avitabile, Acta Crystallogr. Sect. B:
Struct. Crystallogr. Cryst. Chem. B27 (1971) 1859.
[22] F.A. Cotton, M. Jeremic, A. Shaver, Inorg. Chim. Acta 6 (1972)
543.
We gratefully acknowledge the financial support of
the Australian Research Council (DP034270).
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