Preparation, structure and thermal properties of a zinc copper maleate precursor Cu0.06Zn0.94C4O4H2 ·2H2O

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Juraj Černák, Joseph Chomič, Charles Kappenstein and Francis Robert


Abstract

A new Cu–Zn bimetallic precursor Cu0.06Zn0.94C4O4H2 ·2H2O useful as a model catalyst for methanolation of syngas was prepared and identified. It crystallises in the monoclinic space group Cc with cell parameters a = 5.725(1), b = 16.251(2), c = 6.825(1) Å, β = 90.72(1)°, Z = 4. The structure analysis shows a two-dimensional polymeric structure with layers containing metal atoms interconnected by tridentate maleate anions. The smallest ring in the layer contains 18 atoms among which are three metal atoms. These metal atoms are connected by two maleate ligands through the opposite carboxylic groups and the ring is completed by one syn-anti carboxylate bridge Zn–O–C–O–Zn. The metal atom is five-co-ordinated in the MO2O3 form through three oxygen atoms from three different maleate anions and two terminal water ligands. The packing of the structure is stabilised by intra- and inter-layer hydrogen bonds. Thermal decomposition begins with dehydration (75–170 °C) followed by decomposition of the maleate anions (190–635 °C). As final phases, zincite ZnO (major) and tenorite CuO (minor) were identified.


References

  1. Part 4, C. Kappenstein, J. Černák, R. Brahmi, D. Duprez and J. Chomič, Thermochim. Acta, 1996, 279, 65 Search PubMed.
  2. K. C. Waugh, Catal. Today, 1992, 15, 51 CrossRef.
  3. P. B. Rasmussen, P. M. Holmblad, T. Askgaard, C. V. Ovesen, P. Stoltze, J. K. Norskov and I. Chorkendorff, Catal. Lett., 1994, 26, 373 CrossRef CAS.
  4. D. Stirling, F. S. Stone and M. S. Spencer, Proc. 10th International Congress on Catalysis, Budapest, 1992, eds. L. Guczi, F. Solymosi and P. Tétényi, Elsevier, Amsterdam, 1993, pp. 1507–1518 Search PubMed.
  5. P. Porta, S. De Rossi, G. Ferraris and F. Pompa, Solid State Ionics, 1991, 45, 35 CrossRef CAS.
  6. S. V. Ketchik, T. P. Minyukova, L. I. Kuznetsova, L. M. Plyasova, T. M. Yurieva and G. K. Boreskov, React. Kinet. Catal. Lett., 1982, 19, 345 CAS.
  7. L. M. Plyasova, T. M. Yurieva, T. A. Kriger, O. V. Makarova, V. I. Zaikovskij, L. P. Solovieva and A. N. Shmakov, Kinet. Catal. (Engl. Transl.), 1995, 36, 425 Search PubMed and refs. therein.
  8. J. Černák, J. Chomič, C. Kappenstein and M. Dunaj-Jurčo, Z. Krístallogr., 1994, 209, 430 Search PubMed.
  9. J. Černák, C. Kappenstein, Z. Žák and J. Chomič, Acta Crystallogr., Sect. C, 1996, 52, 1067 CrossRef.
  10. J. Černák, J. Chomič, C. Kappenstein, R. Brahmi and D. Duprez, Thermochim. Acta, 1996, 276, 209 CrossRef CAS.
  11. J. R. Allan, G. M. Baillie, J. G. Bonner, D. L. Gerrard and S. Hoey, Thermochim. Acta, 1989, 143, 283 CrossRef CAS.
  12. K. Gora, E. Kyuno and R. Tsuchiya, Bull. Chem. Soc. Jpn., 1968, 41, 2624 CAS.
  13. N. Walker and D. Stuart, Acta Crystallogr., Sect. A, 1983, 39, 158 CrossRef.
  14. D. J. Watkin, J. R. Carruthers and P. W. Betteridge, CRYSTALS User Guide, Chemical Crystallography Laboratory, University of Oxford, 1988 Search PubMed.
  15. P. Ugliendo, G. Borzani and D. Viterbo, J. Appl. Crystallogr., 1988, 21, 75 CrossRef.
  16. C. K. Johnson, ORTEP, Report ORNL-3794, Oak Ridge National Laboratory, Oak Ridge, TN, 1965.
  17. Yu. V. Yablokov, Yu. A. Simonov, M. A. Yampol'skaja, A. A. Dvorkin, G. S. Matuzenko, V. K. Voronkova and L. V. Mosina, Russ. J. Inorg. Chem., 1980, 25, 2468 CAS.
  18. T. Ogata, T. Taga and K. Osaki, Bull. Chem. Soc. Jpn., 1977, 50, 1674 CAS.
  19. M. Horák and D. Papoušek, Infračervená spektra a struktura molekul (IR spectra and structure of molecules), Academia, Praha, 1976 Search PubMed.
  20. A. B. P. Lever, Inorganic Electronic Spectroscopy, Elsevier, Amsterdam, 2nd edn., 1984 Search PubMed.
  21. C. K. Prout, J. R. Carruthers and F. J. C. Rossotti, J. Chem. Soc. A, 1971, 3342 RSC.
  22. A. W. Addison, T. N. Rao, J. Reedijk, J. Van Rijn and G. C. Verschoor, J. Chem. Soc., Dalton Trans., 1984, 1349 RSC.
  23. M. Melnik, K. Györyová, J. Skoršepa and C. E. Holloway, J. Coord. Chem., 1995, 35, 179 CAS.
  24. J. Černák, I. Adzimová, F. Gérard and A. M. Hardy, Acta Crystallogr., Sect. C, 1995, 51, 392 CrossRef.
  25. A. Boultif and D. Louer, J. Appl. Crystallogr., 1993, 26, 140 CrossRef.
  26. R. G. Garvey, Powder Diffr., 1986, 1, 114.
  27. X-Ray Powder Data Files 36-1451 and 41-254, Joint Committee on Powder Diffraction Standards, International Center of Diffraction Data, Swarthmore, PA, 1994.
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