Abstract
Sulfur/oxygen-bridged incomplete cubane-type triphenylphosphine molybdenum and tungsten-clusters [Mo3S4Cl4(H2O)2(PPh3)3]·3THF (1A), [Mo3S4Cl4(H2O)2(PPh3)3]·2THF (2A), [Mo3OS3Cl4(H2O)2(PPh3)3]·2THF (1B), and [W3S4Cl4(H2O)2(PPh3)3]·2THF (1C) were prepared from the corresponding aqua clusters and PPh3 in THF/MeOH. On recrystallization from THF, procedures with and without addition of hexane to the solution gave 1A and 2A, respectively, while the procedures gave no effect on the formation of 1B and 1C. Crystallographic results obtained are as follows: 1A: monoclinic, P21/n, a=17.141(4) Å, b=22.579(5) Å, c=19.069(4) Å, β=96.18(2)°, V=7337(3) Å3, Z=4, R(R w)=0.078(0.102); 1C: monoclinic, P2 1/c, a=12.635(1) Å, b=20.216(4) Å, c=27.815(3) Å, β=96.16(1)°, V=7062(2) Å3, Z=4, R(R w)=0.071(0.083). If the phenyl groups are ignored, the molecule [Mo3S4Cl4(H2O)2(PPh3)3] in 2A has idealized CS symmetry with the mirror plane perpendicular to the plane determined by the metal atoms, while the molecule in 1A does not have the symmetry. The tungsten compound 1C is isomorphous with the molybdenum compound 2A. 31P NMR spectra of 1A, 2A, and 1C were obtained and compared with similar clusters with dmpe (1,2-bis(dimethylphosphino)ethane) ligands.
This is a preview of subscription content, log in via an institution to check access.
Similar content being viewed by others
REFERENCES
(a) F. A. Cotton and G. Wilkinson, Advanced Inorganic Chemistry, 5th ed. (Wiley, New York, 1988), p. 905; (b) V. C. Gibson, C. E. Graimann, P. M. Hare, M. L. H. Green, J. A. Bandy, P. D. Grebenik, and K. Prout (1985). J. Chem. Soc., Dalton Trans. 2025.
(a) F. A. Cotton and R. Llusar (1987). Polyhedron 6, 1741; (b) T. Saito, N. Yamamoto, T. Yamagata, and H. Imoto (1987). Chem. Lett. 2025; (c) F. A. Cotton, P. A. Kibala. M. Matusz, C. S. McCaleb, and R. B. W. Sandor (1989). Inorg. Chem. 28, 2623; (d) Lin Xian-Ti, Shang Mao-Yu, and Huang Jin-Ling (1993). Jiegou Huaxue (J. Struct. Chem.) 12, 155; (e) F. A. Cotton, P. A. Kibala, and C. S. Miertschin (1991). Inorg. Chem. 30, 548.
(a) K. Tsuge, S. Yajima, H. Imoto, and T. Saito (1992). J. Am. Chem. Soc. 114, 7910; (b) K. Tsuge, H. Imoto, and T. Saito (1995). Inorg. Chem. 34, 3404.
V. E. Federov, A. V. Mischchenko, and V. P. Fedin (1985). Russian Chem. Rev 54, 408.
K. Tsuge, H. Imoto, and T. Saito (1992). Inorg. Chem. 31, 4715.
T. Saito, N. Yamamoto, Nagase, T. Tsuboi, K. Kobayashi, T. Yamagata, H. Imoto, and K. Unoura (1990). Inorg. Chem. 29, 764.
S. Kuwata, Y. Mizobe, and M. Hidai (1995). J. Chem. Soc., Chem. Comm. 1057.
(a) T. Saito, Y. Kajitani, T. Yamagata, and H. Imoto (1990). Inorg. Chem. 29, 2951; (b) T. Saito, T. Tsuboi, Y. Kajitani, T. Yamagata, and H. Imoto (1991). Inorg. Chem. 30, 3575.
(a) F. A. Cotton and R. Llusar (1988). Inorg. Chem. 27, 1303; (b) F. A. Cotton and S. K. Mandal (1992). Inorg. Chim. Acta 192, 71; (c) F. A. Cotton, S. K. Mandal, and Maoyu Shang (1990). J. Cluster Sci. 1, 287.
(a) T. Shibahara, M. Yamasaki, G. Sakane, K. Minami, T. Yabuki, and A. Ichimura (1992). Inorg. Chem. 31, 640.
G. M. Sheldrick, Crystallographic Computing 3 G. M. Sheldrick, C. Kruger, and R. Goddard, eds. (Oxford University Press, 1985), p. 175.
Crystal Structure Analysis Package, Molecular Structure Corporation (1985/1992).
F. A. Cotton, R. Llusar, and C. T. Eagle (1989). J. Am. Chem. Soc. 111, 4332.
Author information
Authors and Affiliations
Rights and permissions
About this article
Cite this article
Sasaki, M., Sakane, G., Ouchi, T. et al. Synthesis, Structure, and 31P NMR of Sulfur/Oxygen-Bridged Incomplete Cubane-Type Molybdenum and Tungsten Clusters with Triphenylphosphine Ligands. Journal of Cluster Science 9, 25–43 (1998). https://doi.org/10.1023/A:1022625405761
Issue Date:
DOI: https://doi.org/10.1023/A:1022625405761