Synthesis and characterisation of molybdenum complexes bearing highly functionalised imido substituents[hair space]

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Vernon C. Gibson, Carl Redshaw, William Clegg and Mark R. J. Elsegood


Abstract

The monofunctionalised anilines 2-(H2N)C6H4X (where X = CO2H, SO3H, or CN) reacted with sodium molybdate in the presence of NEt3 and SiMe3Cl in refluxing dme (1,2-dimethoxyethane) to give [NEt3H][MoCl3{2-(HN)C6H4 CO2}{2-Me3SiO2CC 6H4N}] 1, [NEt3H]2[MoCl3{2-NC6H 4SO3}{2-(HN)C6H4 SO3}] 2 and [MoCl2(2-NCC6H4N)2(dme)] 3. Treatment of sodium molybdate with anthranilic acid and 2,6-Pri2C6H3NH2 in a 1∶1 ratio afforded [NEt3H][MoCl3{2-(HN)C6H4 CO2}(NC6H3Pri2-2,6)] 4. Products of reactions of sodium molybdate with the amino acid 2,2-diphenylglycine and 2-aminoterephthalic acid, namely [NEt3H][Mo- Cl3(NCHPh2)(H2NCPh2CO 2)] 5 and [NEt3H][MoCl3{2-HNC6H3 CO2(CO2H)-1,4}{2-NC6H3 (CO2H)2-1,4}] 6 respectively are also reported. Complexes 1 to 6 have been structurally characterised; all contain pseudo-octahedral geometries about the metal centre, and all except 3 are salts in which the anion contains a mer arrangement of chloride ligands.


References

  1. H. H. Fox, K. B. Yap, J. Robbins, S. Cai and R. R. Schrock, Inorg. Chem., 1992, 31, 2287 CrossRef CAS.
  2. P. W. Dyer, V. C. Gibson, J. A. K. Howard, B. Whittle and C. Wilson, J. Chem. Soc., Chem. Commun., 1992, 1666 RSC.
  3. J. H. Oskam, H. H. Fox, K. B. Yap, D. H. McConville, R. O'Dell, B. J. Lichtenstein and R. R. Schrock, J. Organomet. Chem., 1993, 459, 185 CrossRef CAS.
  4. J. B. Arterburn, I. M. Fogarty, K. A. Hall, K. C. Ott and J. L. Bryan, Angew. Chem., 1996, 35, 2877 CAS.
  5. O. D. Sloan and P. Thornton, Polyhedron, 1988, 7, 329 CrossRef CAS.
  6. J. R. Dilworth, V. C. Gibson, C. Lu, J. R. Miller and C. Redshaw, J. Chem. Soc., Dalton Trans., 1997, 269 RSC.
  7. SMART (control) and SAINT (frame integration) software for CCD diffractometers, Siemens Analytical X-ray Instruments, Madison, WI, 1994, together with local programs.
  8. G. M. Sheldrick, SHELXTL, version 5, Siemens Analytical X-Ray Instruments, Madison WI, 1995.
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