Preparation, Characterization And Electrochemical Studies Of 1,1′-bis(diphenylphosphino)ferrocene (dppf) Derivatives. Crystal Structure Of [dppfco(no)2] [sbf6]

The neutral dppfFe(NO)2 (1), the novel cationic [dppfCo(NO)2] [SbF6] (2), as well as the dppfFe(CO)3 (3) (dppf=1,1′-bis-(diphenylphosphino)ferrocene) complexes were prepared and characterized. The interaction between the two metallic centers through the dppf ligand was studied in the solid state by 57Fe Mössbauer spectroscopy and in solution by cyclic voltammetry. The Mössbauer parameters are compared with those of other dppfMLn complexes. Electrochemical studies performed on these complexes show the great influence of the MLn moiety on the redox processes of the dppf iron center. The crystal structure of complex 2 was determined (C34H28CoF6FeN2O2P 2Sb). The compound crystallizes in the triclinic, space group P1̄, a = 10.441(2), b= 10.755(2), c= 17.320(5) Å, α = 104.10(2), β = 0.504(10), γ = 111.504(10)°, U= 1744.7(7) Å3, Z = 2, R = 0.0765, wR2 = 0.1878. In this complex, the cobalt atom is coordinated to two nitrosyl ligands and to phosphorus atoms of the dppf ligand, providing a distorted tetrahedral geometry. © 1997 Elsevier Science S.A.26611927Andy Hor, T.S., Phang, L.-T., (1990) J. Organomet. Chem., 390, p. 345Andy Hor, T.S., Phang, L.-T., (1990) J. Organomet. Chem., 381, p. 121Chan, H.S.O., Andy Hor, T.S., Phang, L.-T., Tan, K.L., (1991) J. Organomet. Chem., 407, p. 353Kim, T.-J., Kwon, S.-C., Kim, Y.H., Heo, N.H., Teeter, M.M., Yamano, A., (1992) J. Organomet. Chem., 426, p. 71Phang, L.-T., Can, K.-S., Lee, H.K., Andy Hor, T.S., (1993) J. Chem. Soc., Dalton Trans., p. 2697Andy Hor, T.S., Chan, H.S.O., Phang, L.-T., Yan, Y.K., Liu, L.-K., Wen, Y.-S., (1991) Polyhedron, 10, p. 2437Yan, Y.K., Chan, H.S.O., Andy Hor, T.S., Tan, K.L., Liu, L.-K., Wen, Y.-S., (1992) J. Chem. Soc., Dalton Trans., p. 423Cramer, E., Percec, V., (1990) Polym. Prepr., Am. Chem. Soc., Div. Polym. Chem., 31, p. 516Kim, T.-J., Kwon, K.-H., Kwon, S.-C., Baeg, J.-O., Shim, S.-C., Lee, D.-H., (1990) J. Organomet. Chem., 389, p. 205Sato, M., Shigeta, H., Sekino, M., Akabori, S., (1993) J. Organomet. Chem., 458, p. 199Munyejabo, V., Damiano, J., Postel, M., Bensimon, C., Roustan, J.L.A., (1995) J. Organomet. Chem., 491, p. 61Andy Hor, T.S., Neo, S.P., Tan, C.S., Mak, T.C.W., Leung, K.W.P., Wang, R.-J., (1992) Inorg. Chem., 31, p. 4510Cuvigny, T., Julia, M., (1986) J. Organomet. Chem., 317, p. 383Cullen, W.R., Kim, T.-J., Einstein, F.W.B., Jones, T., (1985) Organometallics, 4, p. 346Miyaura, N., Ishiyama, T., Sasaki, H., Ishikawa, M., Satoh, M., Suzuki, A., (1989) J. Am. Chem. Soc., 111, p. 314Yuan, K., Scott, W.J., (1991) Tetrahedron Lett., 32, p. 189Castle, P.L., Widdowson, D.A., (1986) Tetrahedron Lett., 27, p. 6013Marr, G., Rockett, B.W., (1990) J. Organomet. Chem., 392, p. 93Houlton, A., Roberts, R.M.G., Silver, J., Parish, R.V., (1991) J. Organomet. Chem., 418, p. 269Housecroft, C.E., Owen, S.M., Raithby, P.R., Shaykh, B.A.M., (1990) Organometallics, 9, p. 1617Watson, W.H., Nagl, A., Hwang, S., Richmond, M.G., (1993) J. Organomet. Chem., 445, p. 163Enemark, J.H., Feltham, R.D., (1974) Coord. Chem. Rev., 13, p. 339Feltham, R.D., (1975) Inorg. Synth., 16, p. 1Leroy, E., Huchette, D., Mortreux, A., Petit, F., (1980) Nouv. J. Chim., 4, p. 173Tkatchenko, I., (1978) J. Mol. Catal., 4, p. 163Ballivet, D., Tkatchenko, I., (1975) J. Mol. Catal., 1, p. 319Mortreux, A., Petit, F., (1986) Appl. Catal., 24, p. 1Pandey, K.K., (1983) Coord. Chem. Rev., 51, p. 69Ballivet, D., Billard, C., Tkatchenko, I., (1977) Inorg. Chim. Acta, 25, pp. L58Huchette, D., Nicole, J., Petit, F., (1979) Tetrahedron Lett., p. 1035Butler, A.R., Williams, D.L.H., (1993) Chem. Soc. Rev., p. 233Keiter, R.L., Keiter, E.A., Hecker, K.H., Boecker, C.A., (1988) Organometallics, 7, p. 2466Gerbase, A.E., Souza, R.F.D., Vichi, E.J.S., Cunha, F.O.V., (1996) Angew. Makrom. Chem., 239, p. 33Ittel, S.D., Tolman, C.A., Krusic, P.J., English, A.D., Jesson, J.P., (1978) Inorg. Chem., 17, p. 3432Ballivet, D., Tkatchenko, I., (1977) Inorg. Chem., 16, p. 945Ballivet-Tkatchenko, D., Billard, C., Revillon, A., (1981) J. Poly. Sci., Poly. Chem. Ed., 19, p. 1697(1992), CAD4, automatic four circle diffractometer, Enraf-Nonius, Delft, Netherlands(1986) Structure Determination Package VAXSDP, Version 3.0, , B.A. Frenz and Associates Inc., College Station, TX and Enraf-Nonius Delft, NetherlandsSheldrick, G.M., (1990) SHELXS86, Program for Crystal Structure Solution, , University of Gottingen, GermanySheldrick, G.M., (1993) SHELXS93, Program for Crystal Structure Solution, , University of Göttingen, GermanyWalker, N., Stuart, D., (1983) Acta Crystallogr., Sect. A, 39, p. 158Bhaduri, S., Grundy, K., Johnson, B.J.G., (1977) J. Chem. Soc., Dalton Trans., p. 2085Bishop, J.J., Davison, A., Katcher, M.L., Lichtenberg, D.W., Merrill, R.E., Smart, J.C., (1971) J. Organomet. Chem., 27, p. 241Corain, B., Longato, B., Favero, G., Ajo, D., Pilloni, G., Russo, U., Kreissl, F.R., (1989) Inorg. Chim. Acta, 157, p. 259Garrou, P.E., (1981) Chem. Rev., 81, p. 229Johnson, C.K., (1965) ORTEP, a Thermal-ellipsoid Plot Program, , Oak Ridge National Laboratory, TNFeltham, R.D., Enemark, J.H., (1981) Top. Stereochem., 12, p. 155Postel, M., Pierrot, M., Wah, H.L.K., (1989) Inorg. Chim. Acta, 165, p. 215Kaduk, J.A., Ibers, J.A., (1977) Inorg. Chem., 16, p. 3283Martin, R.L., Taylor, D., (1976) Inorg. Chem., 15, p. 2970Houlton, A., Ibrahim, S.K., Dilworth, J.R., Silver, J., (1990) J. Chem. Soc., Dalton Trans., p. 2421Crow, J.P., Cullen, W.R., Herring, F.G., Sams, J.R., Tapping, R.L., (1971) Inorg. Chem., 10, p. 1616Mosbaek, H., Poulsen, K.G., (1974) Acta Chem. Scand., Ser. A, 28, p. 157Greenwood, N.N., Gibb, T.C., (1971) Mössbauer Spectroscopy, , Chapman and Hall, LondonSeeber, R., Albertin, G., Mazzochin, G.A., (1982) J. Chem. Soc., Dalton Trans., p. 2561Ramaley, L., Krause, J., (1969) Anal. Chem., 41, p. 1362O'Dea, J.J., Osteryoung, J., Osteryoung, R.A., (1981) Anal. Chem., 53, p. 695Heinze, J., (1984) Angew. Chem., Int. Ed. Engl., 23, p. 831Blanch, S.W., Bond, A.M., Colton, R., (1981) Inorg. Chem., 20, p. 755Baker, P.K., Connelly, N.G., Jones, B.M.R., Maher, J.P., Somers, K.R., (1980) J. Chem. Soc., Dalton Trans., p. 579Chen, H.W., Jolly, W.J., (1979) Inorg. Chem., 18, p. 2549Baker, P.K., Broadley, K., Connelly, N.G., (1982) J. Chem. Soc., Dalton Trans., p. 471Pilloni, G., Longato, B., Corain, B., (1991) J. Organomet. Chem., 420, p. 57Vogler, C., Kaim, W., (1990) J. Organomet. Chem., 398, p. 293Phang, L.-T., Au-Yeung, S.C.F., Andy Hor, T.S., Khoo, S.B., Zhou, Z.-Y., Mak, T.C.W., (1993) J. Chem. Soc., Dalton Trans., p. 165Pilloni, G., Longato, B., (1993) Inorg. Chim. Acta, 208, p. 17Miller, T.M., Ahmed, K.J., Wrighton, M.S., (1989) Inorg. Chem., 28, p. 2347Seller, P., Dunitz, J.D., (1979) Acta Crystallogr., Sect. B, 35, p. 1068Churchill, M.R., Lander, A.G., Rheingold, A.L., (1981) Inorg. Chem., 20, p. 849Geib, S.J., Rheingold, A.L., Dong, T.Y., Heindrickson, D.N., (1986) J. Organomet. Chem., 312, p. 241Cinquantini, A., Opromola, G., Zanello, P.F., Giorgi, G., (1993) J. Organomet. Chem., 444, p. 179. , and Refs. therei