Supertetrahedral sulfide crystals with giant cavities and channels

Science

Volumn 283, Issue 5405, 1999, Pages 1145-1147

  Li, Hailian ^a   Laine, Aaron ^a   O'Keeffe, M ^a   Yaghi, O M ^a  

^a ARIZONA STATE UNIVERSITY   (United States)

Author keywords

[No Author keywords available]

Indexed keywords

SULFIDE; ZEOLITE;

CRYSTALLOGRAPHY; SULFIDE;

ARTICLE; CATALYSIS; CHEMICAL ANALYSIS; CRYSTAL STRUCTURE; CRYSTALLIZATION; PRIORITY JOURNAL; STRUCTURE ANALYSIS;

EID: 0033582633     PISSN: 00368075     EISSN: None     Source Type: Journal    
DOI: 10.1126/science.283.5405.1145     Document Type: Article

References (39)

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23. We have independently made T3 InS materials with the same topology and verified that the largest cavities are very much smaller than in the structures reported here.
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26. J. B. Parise and Y. Ko, Chem. Mater. 6, 718 (1994); see also Parise et al. [J. B. Parise, Y. Ko, K. Tan, D. M. Nellis, S. Koch, J. Solid State Chem. 117, 219 (1995)].
27. 4z)]: In1 (3274, 4448, 1454); In2 (3268, 3357, 1657); In3 (3274, 2260, 1687); In4 (3885, 3885, 0); In5 (3890, 2743, 133); In6 (2746, 2746, 0); S1 (3239, 5000, 2287); S2 (3243, 3938, 2399); S3 (3217, 2815, 2492); S4 (3298, 1702, 2500); S5 (3868, 4471, 708); S6 (3867, 3330, 903); S7 (3876, 2215, 1012); S8 (2734, 4465, 592); S9 (2724, 3340, 775); S10 (2717, 2212, 851). The x-ray data were corrected for absorption, and the structures were solved by direct methods. Sulfur and indium were refined with anisotropic displacement parameters, and the remaining atoms were refined with isotropic parameters. Diffuse electron density (solvent and cations) in the large open volumes was modeled by using Babinet's principle; the atoms thus found in those regions are not necessarily real but serve to account for the residual electron density.
28. Elemental microanalysis for as-synthesized ASU-31: calculated, C, 17.82; H, 3.85; N, 8.91; S, 20.39%; found, C, 17.21; H, 3.26; N, 8.72; S, 20.89%. Elemental microanalysis for as-synthesized ASU-32: calculated, C, 16.48; H, 3.61; N, 3.50; S, 24.01%; found, C, 15.70; H, 3.46; N, 4.19; S, 24.09%. Elemental microanalysis for exchanged ASU-31: found, C, 0.41; H, 1.73; N, 0.55; S, 24.05%. Elemental microanalysis for exchanged ASU-32: found, C, 2.18; H, 1.85; N, 0.70; S, 24.16%. We have some evidence that HPP can act as a dication and give a framework identical to that of ASU-32; thus we allow that some ambiguity in precise determination of the number of HPP guests arises, especially if an ASU-32 framework is also produced in the ASU-31 preparation.
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30. B is often confused with the triclinic form, anorthite, which has the quite different feldspar topology.
31. M. O'Keeffe and O. M. Yaghi, unpublished data.
32. 3 anions. So for n = 1, 3/4 of the ccp sites are occupied. In the limit of n → ∞, 1/16th of the ccp sites are occupied, a 12-fold decrease in density.
33. In calculating the free space we exclude space within a van der Waals radius (1.5 Å for O, 1.8 Å for S, and 2.0 Å for In) of the framework nuclei.
34. Data for VPI-5 are from L. B. McCusker, C. Baerlocher, E. Jahn, M. Bülow, Zeolites 11, 308 (1991); data for a typical faujasite are from M. J. Bennett and J. V. Smith, Mater. Res. Bull. 3, 633 (1968); and data for doverite are from M. Estermann, L. B. McCusker, C. Baerlocher, A. Merrouche, H. Kessler, Nature 352, 320 (1991).
35. Data for VPI-5 are from L. B. McCusker, C. Baerlocher, E. Jahn, M. Bülow, Zeolites 11, 308 (1991); data for a typical faujasite are from M. J. Bennett and J. V. Smith, Mater. Res. Bull. 3, 633 (1968); and data for doverite are from M. Estermann, L. B. McCusker, C. Baerlocher, A. Merrouche, H. Kessler, Nature 352, 320 (1991).
36. Data for VPI-5 are from L. B. McCusker, C. Baerlocher, E. Jahn, M. Bülow, Zeolites 11, 308 (1991); data for a typical faujasite are from M. J. Bennett and J. V. Smith, Mater. Res. Bull. 3, 633 (1968); and data for doverite are from M. Estermann, L. B. McCusker, C. Baerlocher, A. Merrouche, H. Kessler, Nature 352, 320 (1991).
37. For antidots see Weiss et al. [D. Wiess, M. L. Roukes, A. Meuschig, P. Grambow, in Nanostructures and Mesoscopic Systems, W. P. Kirk and M. A. Reed, Eds. (Academic Press, Boston, 1992), p. 299] and Heitmann et al. [D. Heitmann et al., ibid, p. 335].
38. For antidots see Weiss et al. [D. Wiess, M. L. Roukes, A. Meuschig, P. Grambow, in Nanostructures and Mesoscopic Systems, W. P. Kirk and M. A. Reed, Eds. (Academic Press, Boston, 1992), p. 299] and Heitmann et al. [D. Heitmann et al., ibid, p. 335].
39. Financial support from the National Science Foundation (NSF) to M.O.K. (DMR-9804817) and O.M.Y. (CHE-9702131) and continued partial support by Nalco Chemical Company is gratefully acknowledged. We thank F. Hollander for x-ray structure determinations. This research is part of an ongoing effort in the Supramolecular Design and Discovery Group, which is partly supported by the Materials Research Science and Engineering Center of the NSF at Arizona State University.