Facile formation of rare terminal chalcogenido germanium complexes with alkylamidinates as supporting ligands

Journal of the American Chemical Society

Volumn 119, Issue 43, 1997, Pages 10359-10363

  Foley, Stephen R ^a   Bensimon, Corinne ^a   Richeson, Darrin S ^a  

^a UNIVERSITY OF OTTAWA   (Canada)

Author keywords

[No Author keywords available]

Indexed keywords

GERMANIUM DERIVATIVE;

ARTICLE; COMPLEX FORMATION; DRUG SYNTHESIS; IN VITRO STUDY; NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY; REACTION ANALYSIS; X RAY DIFFRACTION;

EID: 0030668296     PISSN: 00027863     EISSN: None     Source Type: Journal    
DOI: 10.1021/ja9719891     Document Type: Article

References (36)

1. For general reviews of multiple bonding to Ge, see: (a) Escudie, J.; Couret, C.; Ranaivonjatovo, H.; Satge, J. Coord. Chem. Rev. 1994, 130, 427.
2. (b) Barrau, J.; Escudie, J.; Satge, J. Chem. Rev. 1990, 90, 283.
3. (c) Baines, K. W.; Stibbs, W. G. Adv. Organomet. Chem. 1996, 39, 275.
4. (a) Tokitoh, N.; Matsumoto, T.; Okazaki, R. J. Am. Chem. Soc. 1997, 119, 2337.
5. (b) Matsumoto, T.; Tokitoh, N.; Okazaki, R. Angew. Chem., Int. Ed. Engl. 1994, 33, 2316.
6. (c) Tokitoh, N.; Matsumoto, T.; Manmaru, K.; Okazaki, R. J. Am. Chem. Soc. 1993, 115, 8855.
7. (d) Tokitoh, N.; Matsuhashi, Y.; Shibata, K.; Matsumoto, T.; Suzuki, H.; Saito, M.; Manmaru, K.; Okazaki, R. Main Group Met. Chem. 1994, 17, 55.
8. (e) Tokitoh, N.; Matsumoto, T.; Ichida, H.; Okazaki, R. Tetrahedron Lett. 1991, 32, 6877.
9. (f) Tokitoh, N.; Saito, M.; Okazaki, R. J. Am. Chem. Soc. 1993, 115, 2065.
10. Veith, M.; Becker, S.; Huch, V. Angew. Chem., Int. Ed. Engl. 1989, 28, 1237.
11. (a) Kuchta, M. C.; Parkin, G. J. Chem. Soc., Chem. Commun. 1996, 1669.
12. (b) Kuchta, M. C.; Parkin, G. J. Chem. Soc., Chem. Commun. 1994, 1351.
13. (c) Kuchta, M. C.; Parkin, G. J. Am. Chem. Soc. 1994, 116, 8372.
14. Ossig, G.; Meller, A.; Bronneke, C.; Muller, O.; Schafer, M.; Herbstinner, R. Organometallics 1997, 16, 2116.
15. Zhou, Y.; Richeson, D. S. J. Am. Chem. Soc. 1996, 118, 10850.
16. 4-] (2.26 Å): Krebs, B. Angew. Chem., Int. Ed. Engl. 1983, 22, 113.
17. 2.
18. Barker, J.; Kilner, M. Coord. Chem. Rev. 1994, 133, 219.
19. Dehnicke, K.; Ergezinger, C.; Hartmann, E.; Zinn, A.; Hösler, K. J. Organomet. Chem. 1988, 352, C1.
20. Roesky, H. W.; Meller, B.; Noltemeyer, M.; Schmidt, H.-G.; Scholz, U.; Sheldrick, G. M. Chem. Ber. 1988, 121, 1403.
21. Ergezinger, C.; Weller, F.; Dehnicke, K. Z. Naturforsch. 1988, 43B, 1621.
22. Kidea, J. D.; Hiller, W.; Borgsen, B.; Dehnicke, K. Z. Naturforsch. 1989, 44B, 889.
23. Appel, S.; Weller, F.; Dehnicke, K. Z. Anorg. Allg. Chem. 1990, 583, 7.
24. Borgsen, B.; Dehnicke, K.; Fenske, D.; Baum, G. Z. Anorg. Allg. Chem. 1991, 596, 133.
25. Kilimann, U.; Noltemeyer, M.; Edelmann, F. T. J. Organomet. Chem. 1993, 443, 35.
26. Edelmann, F. T. Coord. Chem. Rev. 1994, 137, 403.
27. Zhou, Y.; Richeson, D. S. Inorg. Chem. 1997, 36, 501.
28. (a) Zhou, Y.; Richeson, D. S. Inorg. Chem. 1996, 35, 1423.
29. (b) Zhou, Y.; Richeson, D. S. Inorg. Chem. 1996, 35, 2448.
30. The structure of 1 was refined with observed and unobserved reflections to obtain a better ratio of reflections to parameters (2373/298 = 7.96). Although the crystal quality was not ideal, a higher quality crystal was not available. This analysis established the essential molecular structure which was comparable to that of 2. Selected bond distances (Å) and bond angles (deg) for 1: Ge1-N1, 2.037(11); Ge1-N2, 2.158(13); Ge1-N3, 1.935(12); N1-C7, 1.302(19); N2-C7, 1.329(18); N3-C21, 1.364(20); N4-C21, 1.327(18); N1-Ge1-N2, 62.4(4); N1-Ge1-N3, 101.2(5); N2-Ge1-N3, 96.0(4); Ge1-N1-C1, 137.3(10); Ge1-N1-C7, 95.6(9); Ge1-N2-C7, 89.4(9); Ge1-N2-C9, 139.0(9); Ge1-N3-C15, 128.1(10); Ge1-N3-C21, 104.4(9); N1-C7-N2, 111.6(13); N3-C21-N4, 111.4-(12).
31. Selected bond distances (Å) and bond angles (deg) for 2: Ge1-N1, 2.040(9); Ge1-N2, 1.993(10); Ge1-N3, 1.903(9); Ge2-N5, 2.043(9); Ge2-N6, 2.090(9); Ge2-N7, 1.898(9); N1-C7, 1.299(15); N2-C7, 1.420(15); N3-C24, 1.419(15); N4-C24, 1.282(16); N1-Ge1-N2, 65.6(4); N1-Ge1-N3, 107.0(4); N2-Ge1-N3, 108.1(4); Ge1-N1-C1, 129.7(7); Ge1-N1-C7, 93.4(7); Ge1-N2-C7, 91.8(7); Ge1-N2-C12, 135.7(7); Ge1-N3-C18, 133.6(7); Ge1-N3-C24, 112.5-(7); N1-C7-N2, 106.8(10); N3-C24-N4, 125.0(11).
32. Selected bond distances (Å) and bond angles (deg) for 6: Ge-Se, 2.196(4); Ge-N1, 1.86(1); Ge-N3, 2.01(1); Ge1-N4, 1.99(1); N1-C7, 1.42(2); N2-C7, 1.27(2); N3-C24, 1.29(2); N4-C24, 1.35(2); N1-Ge-N3, 106.4(6); N1-Ge-N4, 108.9(6); N3-Ge-N4, 65.6(6); Ge-N1-C7, 119.8(11);C1-N1-C7, 123.9(13); Ge-N3-C24, 92.4(11); Ge-N4-C24, 91.7(11); N3-C24-N4, 109.9(16); Se1-Ge1-N1, 120.0-(5); Se1-Ge1-N3, 122.3(4); Se1-Ge1-N4, 121.4(4).
33. Hitchcock, P. B.; Jang, E.; Lappert, M. F. J. Chem. Soc., Dalton Trans. 1995, 3179. Hitchcock, P. B.; Jasim, H. A.; Lappert, M. F.; Leung, W.-P.; Rai, A. K.; Taylor, R. E. Polyhedron 1991, 10, 1203.
34. Hitchcock, P. B.; Jang, E.; Lappert, M. F. J. Chem. Soc., Dalton Trans. 1995, 3179. Hitchcock, P. B.; Jasim, H. A.; Lappert, M. F.; Leung, W.-P.; Rai, A. K.; Taylor, R. E. Polyhedron 1991, 10, 1203.
35. Selected bond distances (Å) and bond angles (deg) for 10: Ge-Se, 2.2212(3); Ge-N1, 1.9946(15); Ge-N2, 1.9572(15); Ge-N3, 1.8410(15); N1-C7, 1.3367(24); N2-C7, 1.3209(24); N3-S11, 1.7723(15); N3-S12, 1.7542(15); ; Se-Ge-N1, 115.18(5); Se-Ge-N2, 121.03(5); Se-Ge-N3, 120.52(5); N1-Ge-N2, 67.14(6); N1-Ge-N3, 114.05(6); N2-Ge-N3, 107.42(6); Ge-N1-C7, 92.12(11); Ge-N2-C7, 92.06(11);N1-C7-N2, 108.54(16).
36. Fjeldberg, T.; Haaland, A.; Schilling, B. E. R.; Lappert, M. F.; Thorne, A. J. J. Chem. Soc., Dalton Trans. 1986, 1551.