Modular assembly and phase study of two- and three-dimensional porous tin(IV) selenides

Abstract

The work presented focuses attention on a detailed powder and single crystal XRD structure analysis of materials that emerge successively in the hydrothermal synthesis of tetramethylammonium-templated porous tin(IV) selenides. Four phases have been identified in this system and three of them, orthorhombic and monoclinic polymorphs of two-dimensional porous layered TMA₂Sn₃Se₇ (TMA=tetramethylammonium) plus a novel tetragonal three-dimensional open-framework TMA₂Sn₅Se₁₀O have been structurally characterized by single crystal XRD. The order of appearance and interconversion of these materials is shown to follow Oswald's law of successive reactions, which is further supported by Connolly surface calculations. In addition the thermal stability of the orthorhombic TMA₂Sn₃Se₇ phase is explored by in situ variable temperature PXRD under nitrogen and in vacuum, from which it is determined that the structural integrity of the framework is retained up to the point of template removal around 250 and 300 °C, respectively. The accumulated knowledge that has emerged from this study and earlier work allows a modular assembly pathway to be proposed that can rationalize the formation of the observed phases.

References

1. A. R. West, Solid State Chemistry and Its Applications, John Wiley & Sons Ltd., New York, 1989.
2. B. K. Vainshtein, V. M. Fridkin and V. L. Indenbom, Structure of Crystals, Springer-Verlag, New York, 1988.
3. A. R. Verma and P. Krishna, Polymorphism and Polytypism in Crystals, John Wiley & Sons, Inc., New York, 1966.
4. W. Oswald, Z. Phys. Chem., 1897, 22, 289.
5. M. E. Davis and R. F. Lobo, Chem. Mater., 1992, 4, 756.
6. D. Turnbull, Phase Changes, in Solid State Physics, ed. F. Seitz and D. Turnbull, Academic Press, New York, 1956.
7. L. S. Ramsdell, Am. Mineral., 1945, 30, 519.
8. D. W. Breck, Zeolites Molecular Sieves, Structure, Chemistry and Use, John Wiley and Sons, New York, 1974.
9. R. F. Adamsky and K. M. Merz, Z. Kristallogr., 1959, 111, 350.
10. G. Honjo, S. Miyake and T. Tomita, Acta Crystallogr., 1950, 3, 396.
11. B. Palosz, W. Palosz and S. Gierlotka, Acta Crystallogr., Sect. C, 1985, 41, 807.
12. B. Palosz, W. Palosz and S. Gierlotka, Acta Crystallogr., Sect. C, 1985, 41, 1402.
13. B. Palosz, W. Palosz and S. Gierlotka, Acta Crystallogr., Sect. C, 1986, 42, 653.
14. A. R. Verma, Proc. R. Soc. London, Ser. A, 1952, 65, 525.
15. R. S. Mitchel, Z. Kristallogr., 1957, 109, 1.
16. A. R. Verma and P. Krishna, Proc. R. Soc. London, Ser. A, 1957, 240, 462.
17. B. Palosz, Phys. Status Solidi A, 1983, 80, 11 and references therein.
18. B. Palosz and S. Gierlotka, Acta Crystallogr., Sect. C, 1985, 1404.
19. D. I. Bletskan, I. M. Mitrovtsii, V. A. Stefanovich, M. V. Portorii, Yu. V. Voroshilov and V. Yu. Slivka, Sov. Phys. Crystallogr., 1987, 32, 224.
20. C. L. Bowes, Ph.D Thesis, University of Toronto, 1996.
21. T. Jiang, Ph.D Thesis, University of Toronto, 1997.
22. T. Jiang, A. L. Lough, G. A. Ozin, D. Young and B. L. Bedard, Chem. Mater., 1995, 2, 245.
23. G. A. Ozin, Supramol. Chem., 1995, 6, 125.
24. H. Ahari, Ö. Dag, S. Petrov, G. A. Ozin and R. L. Bedard, J. Phys. Chem., 1998, 102, 2356.
25. Cerius2 Simulation Tools User's Reference, BIOSYM/Molecular Simulations, 1995, p. 195.
26. H. Ahari, R. L. Bedard, C. Bowes, N. Coombs, Ö. Dag, T. Jiang, G. A. Ozin, S. Petrov, A. Verma, G. Vovk and D. Young, Nature, 1997, 388, 857.
27. C. L. Bowes, S. Petrov, G. Vovk, D. Young and G. A. Ozin, J. Mater. Chem., 1998, 8, 711.
28. W. S. Sheldrick and H. G. Braunbeck, Z. Naturforsch., Teil B, 1990, 45, 1643.
29. J. B. Parise, Y. Ko, K. Tan, D. M. Nellis and S. J. Koch, J. Solid State Chem., 1995, 117, 219.
30. A. Blecher, M. Dräger and B. Mathiasch, Z. Naturforsch., Teil B, 1981, 86, 1361.
31. O. M. Yaghi, Z. Sun, D. A. Richardson and T. L. Groy, J. Am. Chem. Soc., 1994, 116, 807.
32. O. M. Yaghi, D. A. Richardson, C. E. Davis, G. Li and T. L. Groy, Mater. Res. Symp. Proc., 1995, 371, 15.
33. M. Ribes, J. Oliver-Fourcade, E. Philippot and M. Maurin, J. Solid State Chem., 1973, 8, 195.
34. H. Ahari and G. A. Ozin, 1997, unpublished results.
35. B. Krebs and S. Pohl, Z. Naturforsch., Teil B, 1971, 26, 853.
36. B. Krebs and S. Pohl, Z. Anorg. Allg. Chem., 1976, 424, 265.
37. B. Krebs and W. Schiwy, Angew. Chem., Int. Ed. Engl., 1975, 14, 261.
38. B. Krebs, Angew. Chem., Int. Ed. Engl., 1983, 22, 113.
39. W. M. Meier and D. H. Olson, Atlas of Zeolite Structure Types, Butterworth-Heinemann, London, 3rd revised edn., 1992.
40. M. L. Connolly, J. Appl. Crystallogr., 1983, 16, 548.
41. M. L. Connolly, Science, 1983, 221, 709.
42. T. Jiang, G. A. Ozin and R. L. Bedard, Adv. Mater., 1995, 7, 166.
43. T. Jiang, G. A. Ozin and R. L. Bedard, Adv. Mater., 1994, 6, 860.
44. B. Krebs, Angew. Chem., Int. Ed. Engl., 1983, 22, 113 and references therein.
45. B. Krebs and H.-U. Hürter, Z. Anorg. Allg. Chem., 1980, 462, 143.
46. W. S. Sheldrick and B. Schaaf, Z. Anorg. Allg. Chem., 1994, 620, 1041.
47. W. S. Sheldrick and H. G. Braunbeck, Z. Naturforsch., Teil B, 1989, 44, 851.
48. B. Krebs and S. Pohl, Z. Anorg. Allg. Chem., 1972, 241, 393.
49. D. Young and G. A. Ozin, 1995, unpublished results.
50. Ö. Yükseker, A. L. Lough and G. A. Ozin, 1997, unpublished results.
51. I. D. Gay, C. H. W. Jones and R. D. Sharma, J. Man. Reson., 1989, 84, 501.