Abstract
The reaction of Ru3(CO)12 and [Ir(CO)4]- (as [PPh4]+ or [N(PPh3)2]+ salts) yields the anion [Ru3Ir2(CO)14]2- (1) which has been found to derive from the intermediate [Ru3Ir(CO)13]- anion. Treatment of (1) with acids gives the conjugated hydrido species [Ru3Ir2(CO)14H]- (2). The two anions were characterized by single-crystal X-ray diffraction of their [PPh4]+ salts. [PPh4]2[Ru3Ir2(CO)14]: space group C2/c, Z=4, a=22.121(5) Å, b=10.546(5) Å, c=25.931(5) Å, β=103.870(5)°, R=0.052 and Rw=0.130 for 3128 independent reflections with I>2σ(I ). [PPh4][Ru3Ir2(CO)14H]: space group P21/c, Z=8, a=22.833(5) Å, b=13.893(5) Å, c=25.810(5) Å, β=92.650(5)°, R=0.070 and Rw=0.150 for 12141 independent reflections with I>2σ(I). Both anions 1 and 2 have a trigonal bipyramidal metal frame. There are two independent anions in the asymmetric unit of 2 differing in their ligand stereochemistry.
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REFERENCES
A. Fumagalli, T. F. Koetzle, and F. Takusagawa (1981). J. Organometal. Chem. Chini Mem. Issue 213, 365.
A. Fumagalli, F. Demartin, and A. Sironi (1985). J. Organometal. Chem. 279, C33.
A. Fumagalli and G. Ciani (1984). J. Organometal. Chem. 272, 91
A. Fumagalli, M. C. Malatesta, and A. Sironi, unpublished results; D. Italia, Tesi di Laurea in Chimica, a.a. (1993)–(1994).
R. Della Pergola, L. Garlaschelli, F. Demartin, M. Manassero, N. Masciocchi, M. Sansoni, and A. Fumagalli (1989). J. Chem. Soc. Dalton Trans. 1109.
P. Macchi, D. M. Proserpio, and A. Sironi (1997). Organometallics 16, 2101
(a) [Ir6(CO)16]: L. Garlaschelli, S. Martinengo, P. L. Bellon, F. Demartin, M. Manassero, M. Y. Chiang, C. Wei, and R. Bau (1984). J. Am. Chem. Soc. 106, 6664. (b) [Ru6C(CO)16]2– (C2v —[AsPh4]+ salt): B. F. G. Johnson, J. Lewis, S. W. Sankey, K. Wong, M. McPartlin, and W. J. H. Nelson (1980). J. Organomet. Chem. 191, C3.n (C __S [NEt4]+ salt): J. S. Bradley, G. B. Ansell, and E. W. Hill (1980). J. Organomet. Chem. 184, C33; G. B. Ansell and J. S. Bradley (1980). Acta Cryst. B 36, 726. (c) [H3Ru4(CO)12]-: M. McPartlin and W. J. H. Nelson (1986). J. Chem. Soc. Dalton 1557, and refs. therein. (d) [Rh11(CO)23]3-: A. Fumagalli, S. Martinengo, G. Ciani, A. Sironi, and B. T. Heaton (1988). J. Chem. Soc. Dalton 163. (e) [Fe4(CO)13]2- ([Fe(Py)6]2+ salt): R. J. Doedens and L. F. Dahl (1966). J. Amer. Chem. Soc. 88, 4847. ([PPN]+ salt): G. van Buskirk, C. B. Knobler, and H. D. Kaesz (1985). Organometallics 4, 149. (f ) [Ru6C(CO)17]: D. Braga, F. Grepioni, P. J. Dyson, B. F. G. Johnson, P. Frediani, M. Bianchi, and F. Piacenti (1992). J. Chem. Soc. Dalton 2565, and refs. therein. (g) [Fe5N(CO) 14]-: R. Hourihane, T. R. Spalding, G. Ferguson, T. Deeney, and P. Zanello (1993). J. Chem. Soc. Dalton 43. (h) [Cr2(CO)10]2- ([2,2,2-Crypt-Na]+ salt): H. Borrmann, A. M. Pirani, and G. J. Schrobilgen (1997). Acta. Cryst. C 53, 19. ([2,2,2-Crypt-K]+ salt): H. Borrmann, A. M. Pirani, and G. J. Schrobilgen (1997). Acta. Cryst. C 53, 1007, and refs. therein.
A. Sironi, in Braunstein, Oro, and Raithby (eds.), Metal Clusters in Chemistry. Vol. 2 (Wiley, VCH, 1999), pp. 937–959.
A. G. Orpen (1980). J. Chem. Soc. Dalton Trans. 2509.
L. Garlaschelli, R. Della Pergola, and S. Martinengo (1991). Inorg. Synth. 28, 211.
A. C. North, D. C. Phillips, and F. S. Mathews (1968). Acta Crystallogr. A 24, 351.
A. Altomare, G. Cascarano, C. Giacovazzo, A. Guagliardi, M. C. Burla, G. Polidori, and M. Camalli (1994). J. Appl. Crystallogr. 24, 435.
G. M. Sheldrick, SHELX97-Program for the Refinement of Crystal Structure (University of Göttingen, Göttingen, Germany, 1997).
G. M. Sheldrick, SADABS (University of Göttingen, Göttingen, Germany, 1996).
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Fumagalli, A., Malatesta, M.C., Vallario, M. et al. Mixed Ruthenium–Iridium Carbonyl Cluster Complexes. Synthesis of the Anions [Ru3Ir2(CO)14]2− and [Ru3Ir2(CO)14H]− and Crystal Structures of Their [tetraphenylphosphonium]+ Salts. Journal of Cluster Science 12, 187–200 (2001). https://doi.org/10.1023/A:1016631314528
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DOI: https://doi.org/10.1023/A:1016631314528