View PDF Version
 
DOI: 10.1039/A807816E (Paper) Reference Section for: J. Chem. Soc., Dalton Trans., 1999, 987-996

Synthesis and crystal structures of mononuclear half-sandwich complexes of Ni and Co containing Kläui’s tripodal ligand, [M{κ3-(η5-C5H5)Co[P([double bond, length half m-dash]O)(OCH3)2]3}(κ2-NO3)(L)] (M = Ni or Co)

(Note: The full text of this document is currently only available in the PDF Version )

Munetaka Akita, De-qiang Ma, Shiro Hikichi and Yoshihiko Moro-oka

Abstract

Synthesis of LORM–X-type 1∶1 mononuclear adducts containing Kläui’s tripodal ligands {LOR = CpCo[P([double bond, length half m-dash]O)(OR)2]3} was studied. Addition of NaLOMe to an excess amount of CoCl2 did not afford a mononuclear product but the dinuclear complex [Co(µ-LOMe)2CoCl2] 1, which results from co-ordination of the two P[double bond, length half m-dash]O oxygen atoms in the initially formed 1∶2 adduct, Co(LOMe)2, to a second molecule of CoCl2. In contrast, similar reaction of nitrate salts M(NO3)2·6H2O followed by crystallization from acetone produced 1∶1 mononuclear complexes, [MLOMe(κ2-NO3)(Me2CO)] M = Ni 3 or Co 4], with octahedral co-ordination geometry. Before crystallization from acetone the dinuclear adduct [Ni(µ-LOR)2(µ-NO3)2Ni(NO3)] 2 was isolated from a reaction mixture and subsequent treatment with acetone gave the mononuclear product 3. Thus, for synthesis of LORM–X-type complexes, it is essential to use a potentially κ2-co-ordinating ligand (e.g. NO3) in the presence of a donor (e.g. acetone). The labile acetone ligand in 3 is replaced by P- and N-donors to give the substituted products [NiLOMe(κ2-NO3)(L)] (L = PPh3 5a, 2,5-dimethylpyridine 5b or 3,5-diisopropylpyrazole 5c) and [NiLOMe(κ2-NO3)(py)3]NO3 6. Complexes 1, 2b, 2c, 3, 4, 5a–5c, 6, and [NiLOMe(κ2-NO3)(MeOH)] were characterized by X-ray crystallography.

References

  1. Reviews: S. Trofimenko, Chem. Rev., 1993, 93, 943 Search PubMed; N. Kitajima and W. B. Tolman, Prog. Inorg. Chem., 1995, 43, 419 CrossRef CAS; N. Kitajima and Y. Moro-oka, Chem. Rev., 1994, 94, 737 CAS.
  2. Reviews: K. Wieghardt and P. Chaudhury, Prog. Inorg. Chem., 1988, 35, 329 Search PubMed; W. B. Tolman, Acc. Chem. Res., 1997, 30, 227 Leading references: J. R. Hartman, R. L. Radin, P. Chauduri, K. Pohl, K. Wieghardt, B. Nuber, J. Weiss, G. C. Papefthymiou, R. B. Frankel and S. J. Lippard, J. Am. Chem. Soc., 1987, 109, 7387 CrossRef CAS; P. Chauduri, M. Winter, K. Wieghardt, S. Gehring, W. Haase, B. Nuber and J. Weiss, Inorg. Chem., 1988, 27, 1564 Search PubMed; S. Drüeke, K. Wieghardt, B. Nuber and J. Weiss, Inorg. Chem., 1989, 28, 1414 CrossRef CAS; U. Bossek, T. Weyermüller, K. Wieghardt, J. Bonvoisin and J. J. Girerd, J. Chem. Soc., Chem. Commun., 1989, 633 CrossRef CAS; P. Chaudhuri, M. Winter, D. Védova, P. Fleischhauer, W. Haase, U. Flörke and H.-J. Haupt, Inorg. Chem., 1991, 30, 4777 CrossRef CAS; R. Hotzelmann, K. Wieghardt, J. Ensling, H. Romstedt, P. Gütlich, E. Bill and H.-J. Haupt, J. Am. Chem. Soc., 1992, 114, 9470 RSC; R. Hotzelmann, K. Wieghardt, U. Flörke, H.-J. Haupt, D. C. Weatherburn, J. Bonviosin, G. Blondin and J.-J. Girerd, J. Am. Chem. Soc., 1992, 114, 1681 CrossRef CAS; L. Wang and T. C. Flood, J. Am. Chem. Soc., 1992, 114, 3169 CrossRef CAS; T. N. Margulis and L. J. Zompa, Inorg. Chim. Acta, 1992, 201, 61 CrossRef CAS; D. Hanke, K. Wieghardt, B. Nuber, R.-S. Lu, R. K. McMullan, T. F. Koetzle and B. Bau, Inorg. Chem., 1993, 32, 4300 CrossRef CAS; F. Birkelbach, M. Winter, U. Flörke, H.-J. Haupt, C. Butxlaff, M. Lengen, E. Bill, A. X. Trautwein, K. Wieghardt and P. Chaudhuri, Inorg. Chem., 1994, 33, 3990 CrossRef CAS; Y. Sasaki, K. Umakoshi, S. Kimura, C.-E. Oh, M. Yamazaki and T. Shibahara, Chem. Lett., 1994, 1185 CrossRef CAS; L. Wang, C. Wang, R. Bau and T. C. Flood, Organometallics, 1996, 15, 491 CrossRef CAS; S.-M. Yang, M. C.-W. Chan, K.-K. Cheung, C.-M. Che and S.-M. Peng, Organometallics, 1997, 16, 2819 CAS; J. A. Halfen, S. Maharatra, E. C. Wilkinson, E. C. Kaderli, V. G. Young, Jr., L. Que, Jr., A. D. Zuberbühler and W. B. Tolman, Science, 1996, 271, 1397 CrossRef CAS; S. Maharatra, J. A. Halfen, E. C. Wilkinson, G. Pan, V. G. Young, Jr., C. J. Cramer, L. Que, Jr. and W. B. Tolman, J. Am. Chem. Soc., 1996, 118, 11555 CrossRef.
  3. (a) M. Akita, K. Ohta, Y. Takahashi, S. Hikichi and Y. Moro-oka, Organometallics, 1997, 16, 4121 CrossRef CAS; (b) Y. Takahashi, M. Akita, S. Hikichi and Y. Moro-oka, Inorg. Chem., 1998, 37, 2614 CrossRef CAS; (c) Y. Takahashi, M. Akita, S. Hikichi and Y. Moro-oka, Organometallics, 1998, 37, 4884 CrossRef CAS; (d) M. Akita, T. Miyaji, S. Hikichi and Y. Moro-oka, Chem. Commun., 1998, 1005 RSC; (e) S. Hikichi, H. Komatsuzaki, N. Kitajima, M. Akita, M. Mukai, T. Kitagawa and Y. Moro-oka, Inorg. Chem., 1997, 36, 266 CrossRef CAS; (f) S. Hikichi, H. Komatsuzaki, M. Akita and Y. Moro-oka, J. Am. Chem. Soc., 1998, 120, 4699 CrossRef CAS; (g) S. Hikichi, M. Yoshizawa, Y. Sasakura, M. Akita and Y. Moro-oka, J. Am. Chem. Soc., 1998, 120, 10567 CrossRef CAS; (h) M. Akita, N. Shirasawa, S. Hikichi and Y. Moro-oka, Chem. Commun., 1998, 973 RSC; (i) T. Ogihara, S. Hikichi, M. Akita and Y. Moro-oka, Inorg. Chem., 1998, 37, 2614 CrossRef CAS; (j) H. Komatsuzaki, Y. Nagasu, K. Suzuki, T. Shibasaki, M. Satoh, F. Ebina, S. Hikichi, M. Akita and Y. Moro-oka, J. Chem. Soc., Dalton Trans., 1998, 511 RSC; (k) H. Komatsuzaki, S. Ichikawa, S. Hikichi, M. Akita and Y. Moro-oka, Inorg. Chem., 1998, 37, 3652 CrossRef CAS; (l) M. Akita, K. Fujisawa, S. Hikichi and Y. Moro-oka, Res. Chem. Interm., 1998, 24, 291 Search PubMed.
  4. W. Kläui, Angew. Chem., Int. Ed. Engl., 1990, 29, 627 CrossRef.
  5. J. P. Jesson, S. Trofimenko and D. R. Eaton, J. Am. Chem. Soc., 1967, 89, 3148 CrossRef CAS; Comprehensive Organometallic Chemistry II, eds. E. W. Abel, F. G. A. Stone and G. Wilkinson, Pergamon, Oxford, 1995 Search PubMed.
  6. U. Siemeling, U. Vorfeld, R. Neumann and H. Stammler, Organometallics, 1998, 17, 483 CrossRef CAS.
  7. (a) R. Han and G. Parkin, J. Am. Chem. Soc., 1991, 113, 9707 CrossRef CAS; (b) R. Han, A. Looney, K. McNeill, G. Parkin, A. L. Rheingold and B. S. Haggerty, J. Inorg. Biochem., 1993, 49, 105 CrossRef CAS; (c) A. Looney and G. Parkin, Inorg. Chem., 1994, 33, 1234 CrossRef CAS; (d) A. Looney, A. Saleh, Y. Zhang and G. Parkin, Inorg. Chem., 1994, 33, 1158 CrossRef CAS; (e) N. V. P. Kumar and D. S. Marynick, Inorg. Chem., 1993, 32, 1857 CrossRef; (f) R. Alsfasser, A. K. Powell, S. Trofimenko and H. Vahrenkamp, Chem. Ber., 1993, 126, 685 CAS; (g) T. Tanase, J. W. Yun and S. J. Lippard, Inorg. Chem., 1995, 34, 4220 CrossRef CAS; (h) J. W. Yun, T. Tanase, L. E. Pence and S. J. Lippard, J. Am. Chem. Soc., 1995, 117, 4407 CrossRef CAS; (i) C. He and S. J. Lippard, J. Am. Chem. Soc., 1998, 120, 105 CrossRef CAS; (j) N. Kitajima, S. Hikichi, M. Tanaka and Y. Moro-oka, J. Am. Chem. Soc., 1993, 115, 5496 CrossRef CAS.
  8. W. Kläui, B. Lenders, B. Hessner and K. Evertz, Organometallics, 1988, 7, 1357 CrossRef; B. Lenders, W. Kläui, M. Irmler and G. Meyer, J. Chem. Soc., Dalton Trans., 1990, 2069 RSC; W. Kläui and B. Lenders, Chem. Ber., 1990, 123, 2233 CAS; X. Feng, S. G. Bott and S. J. Lippard, J. Am. Chem. Soc., 1989, 111, 8046 CrossRef CAS; M. Scotti, M. Valderrama, S. Rojas and W. Kläui, J. Organomet. Chem., 1986, 301, 369 CrossRef CAS; W. Kläui, M. Scotti, M. Valderrama, S. Rolas, G. M. Sheldrick, P. G. Jones and T. Scroeder, Angew. Chem., Int., Ed. Engl., 1985, 24, 683 CrossRef; W. Kläui, H. Otto, W. Eberspach and E. Buchholz, Chem. Ber., 1982, 115, 1922; J. M. Power, K. Everttz, L. Henling, R. Marsh, W. P. Schaefer, J. A. Labinger and J. E. Bercaw, Inorg. Chem., 1990, 29, 5058 CrossRef CAS; E. Kelson, L. Henling, W. P. Schaefer, J. A. Labinger and J. E. Bercaw, Inorg. Chem., 1993, 32, 2863 CrossRef CAS; U. Kölle, G. Flunkert, R. Görissen, M. Schmidt and U. Englert, Angew. Chem., Int. Ed. Engl., 1992, 31, 440 CrossRef; W.-H. Leung, E. Y. Y. Chan, I. D. Williams and W. T. Wong, Organometallics, 1997, 16, 3234 CrossRef CAS; T. R. Ward, S. Duclos, B. Therrien and K. Schenk, Organometallics, 1998, 17, 2490 CrossRef CAS; W. Kläui, A. Müller, W. Eberspach, R. Bose and I. Goldberg, J. Am. Chem. Soc., 1987, 109, 164 CrossRef; W. Kläui and H. Hamers, J. Organomet. Chem., 1988, 345, 287 CrossRef; W. Kläui and T. Hardt, J. Organomet. Chem., 1996, 526, 313 CrossRef; W. Kläui, T. Hardt, H.-J. Schulte and H. Hamers, J. Organomet. Chem., 1995, 498, 63 CrossRef; W. Kläui, M. Glaum, T. Wagner and M. A. Bennett, J. Organomet. Chem., 1994, 472, 355 CrossRef; B. Domhöver, H. Hamers, W. Kläui and M. Pfeffer, J. Organomet. Chem., 1996, 522, 197 CrossRef; B. Domhöver and W. Kläui, J. Organomet. Chem., 1996, 522, 207 CrossRef.
  9. E. Dubler, L. Linowsky and W. Kläui, Transition Met. Chem., 1979, 4, 191 CAS.
  10. C. K. Johnson, ORTEP, Report ORNL-5138, Oak Ridge National Laboratory, Oak Ridge, TN, 1976.
  11. O. Krampe, C.-E. Song and W. Kläui, Organometallics, 1993, 12, 4949 CrossRef CAS.
  12. W. Kläui, H.-O. Asbahr, G. Schramm and U. Englert, Chem. Ber., 1997, 130, 1223 CAS.
  13. D. Stuart and N. Walker, Acta Crystallogr., Sect. A, 1979, 35, 925 CrossRef CAS.
  14. TEXSAN, Crystal Structure Analysis Package, Molecular Structure Corporation, Houston, TX, 1985 and 1992.
  15. International Tables for X-Ray Crystallography, Kynoch Press, Birmingham, 1975, vol. 4 Search PubMed.
  16. G. M. Sheldrick, SHELXS 86, University of Göttingen, 1986.
  17. P. T. Beurskens, G. Admiraal, G. Buerskens, W. P. Bosman, S. Garcia-Granda, R. O. Gould, J. M. M. Smits and C. Smykalla, DIRDIF 92, Technical Report of the Crystallographic Laboratory, University of Nijmegen, 1992.
  18. G. M. Sheldrick, SHELXL 93, University of Göttingen, 1993.
Click here to see how this site uses Cookies. View our privacy policy here.