Two-dimensional polytypism of "crystalline" (C5Me5)ReO3

Inorganic Chemistry

Volumn 35, Issue 13, 1996, Pages 4060-4063

  Masciocchi, Norberto ^a   Cairati, Paolo ^a   Saiano, Filippo ^b   Sironi, Angelo ^a  

^a UNIVERSITY OF MILAN   (Italy)

^b UNIVERSITY OF PALERMO   (Italy)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 0041540851     PISSN: 00201669     EISSN: None     Source Type: Journal    
DOI: 10.1021/ic951502u     Document Type: Article

References (37)

1. Burrell, A. K.; Cotton, F. A.; Daniels, L. M.; Petricek, V. Inorg. Chem. 1995, 34, 4253.
2. Herrmann, W. A.; Serrano, R.; Bock, H. Angew. Chem. Int. Ed. Engl. 1984, 23, 383.
3. (a) Herrmann, W. A.; Hardtweck, E.; Floel, M.; Kulpe, J.; Küsthardt, U.; Okuda, J. Polyhedron 1987, 6, 1165.
4. (b) Herrmann, W. A. J. Organomet. Chem. 1986, 300, 111.
5. Herrmann, W. A. Angew. Chem., Int. Ed. Engl. 1988, 27, 1297. Herrmann, W. A.; J. Organomet. Chem. 1990, 382, 1.
6. Herrmann, W. A. Angew. Chem., Int. Ed. Engl. 1988, 27, 1297. Herrmann, W. A.; J. Organomet. Chem. 1990, 382, 1.
7. (a) Herrmann, W. A.; Serrano, R.; Schafer, A.; Küsthardt, U.; Ziegler, M L.; Guggolz, E. J. Organomet. Chem. 1984, 272, 55.
8. (b) Okuda, K., Hardtweck, E.; Herrmann, W. A. Inorg. Chem. 1988, 27, 1254.
9. (c) Herrmann, W. A.; Alberto, R.; Kiprof, P.; Baumgartner, F.; Angew. Chem., Int. Ed. Engl. 1990, 29, 189.
10. Kanellakopulos, B.; Nuber, B.; Raptis, K.; Ziegler, M. Angew. Chem., Int. Ed. Engl. 1989, 28, 1055.
11. Masciocchi, N.; Cairati, P., Sironi, A. Book of Abstracts: ACA Annual Meeting, Albuquerque, NM, 1993; ACA: Storrs, CT, 1993; S004, p 47.
12. Patton, A T.; Strouse, C. E.; Knobler, C. B.; Gladysz, J. A. J. Am. Chem. Soc. 1983, 105, 5804.
13. Herrmann, W. A.; Voss, E., Floel, M. J. Organomet. Chem 1985, 297, C5.
14. North, A. C. T.; Phillips, D. C.; Mathews, F. S. Acta Crystallogr. 1968, A24, 351.
15. The twinning plane, following Burrell's formulation, is [100].
16. This model could be (very slightly) improved by considering racemic twins (with domains differing in their anomalous scattering contribution).
17. Sheldrick, G. M. SHELX 93: A program for crystal structure refinement; University of Göttingen: Göttingen Germany, 1993.
18. It is well-known that the simultaneous sampling of all reciprocal lattice nodes having the same 2θ makes the powder diffraction technique poorer (compared to standard single-crystal analysis), because severe (accidental or exact) overlaps of peaks occur. For the very same reason, however, (macro)twinning, i.e. the presence of two (or more) ordered macroscopic domains within each crystallite, does not affect the powder patterns, as long as preferred orientation of the crystallites is avoided (Li, J.; McCulley, F ; McDonnell, S. L.; Masciocchi, N.; Proserpio, D. M.; Sironi, A. Inorg. Chem. 1993, 32, 4829). In particular, the powder spectrum of the title compound shows the following: (i) the presence at low angles of broad, but well-defined, peaks (100 and 120) which are forbidden in Pmnm; (ii) a marked asymmetric broadening of some peaks (counterparted, in the "single-crystal" data collection, by anomalous peak widths of 1.8-2.0°); (iii) a structured background level. These features, which correspond to the streaks observed by Burrell on oscillation photographs, cannot be accounted for by ordinary twinning but are indicative of the paracrystalline and/or faulted nature of the crystals ( Guimer, A. X-ray Diffraction in Crystals, Imperfect Crystals and Amorphous Bodies; Freeman & Co.: San Francisco, CA, 1963. Reynolds, R. C. In Modern Powder Diffraction; Bish, D. L., Post, J. E., Eds.; Reviews in Mineralogy, 20.; The Mineralogical Society of America: Washington, DC, 1989; p 145). Consistently, we failed to satisfactory reproduce all such features by using, in a Rietveld refinement, any of the four structural models presented in the single-crystal analysis. However, some of these anomalies can be reproduced by our faulted model: (a) on nanocrystals, by the Debye interference function (Espinat, D.; Thevenot, F.; Grimound, J.; El Malki, K. J. Appl. Crystallogr. 1993, 26, 368) (b) on nanocrystals, by the explicit Fourier transform (Neder, R. B. Z. Kristallogr. 1994, Suppl. 8, 744); on infinitely thick crystals, by recursive algorithms (Treacy, M. M. J.; Newsam, J. M.; Deem, M. W. Proc. R. Soc. London, A 1991, 433, 499).
19. It is well-known that the simultaneous sampling of all reciprocal lattice nodes having the same 2θ makes the powder diffraction technique poorer (compared to standard single-crystal analysis), because severe (accidental or exact) overlaps of peaks occur. For the very same reason, however, (macro)twinning, i.e. the presence of two (or more) ordered macroscopic domains within each crystallite, does not affect the powder patterns, as long as preferred orientation of the crystallites is avoided (Li, J.; McCulley, F ; McDonnell, S. L.; Masciocchi, N.; Proserpio, D. M.; Sironi, A. Inorg. Chem. 1993, 32, 4829). In particular, the powder spectrum of the title compound shows the following: (i) the presence at low angles of broad, but well-defined, peaks (100 and 120) which are forbidden in Pmnm; (ii) a marked asymmetric broadening of some peaks (counterparted, in the "single-crystal" data collection, by anomalous peak widths of 1.8-2.0°); (iii) a structured background level. These features, which correspond to the streaks observed by Burrell on oscillation photographs, cannot be accounted for by ordinary twinning but are indicative of the paracrystalline and/or faulted nature of the crystals ( Guimer, A. X-ray Diffraction in Crystals, Imperfect Crystals and Amorphous Bodies; Freeman & Co.: San Francisco, CA, 1963. Reynolds, R. C. In Modern Powder Diffraction; Bish, D. L., Post, J. E., Eds.; Reviews in Mineralogy, 20.; The Mineralogical Society of America: Washington, DC, 1989; p 145). Consistently, we failed to satisfactory reproduce all such features by using, in a Rietveld refinement, any of the four structural models presented in the single-crystal analysis. However, some of these anomalies can be reproduced by our faulted model: (a) on nanocrystals, by the Debye interference function (Espinat, D.; Thevenot, F.; Grimound, J.; El Malki, K. J. Appl. Crystallogr. 1993, 26, 368) (b) on nanocrystals, by the explicit Fourier transform (Neder, R. B. Z. Kristallogr. 1994, Suppl. 8, 744); on infinitely thick crystals, by recursive algorithms (Treacy, M. M. J.; Newsam, J. M.; Deem, M. W. Proc. R. Soc. London, A 1991, 433, 499).
20. It is well-known that the simultaneous sampling of all reciprocal lattice nodes having the same 2θ makes the powder diffraction technique poorer (compared to standard single-crystal analysis), because severe (accidental or exact) overlaps of peaks occur. For the very same reason, however, (macro)twinning, i.e. the presence of two (or more) ordered macroscopic domains within each crystallite, does not affect the powder patterns, as long as preferred orientation of the crystallites is avoided (Li, J.; McCulley, F ; McDonnell, S. L.; Masciocchi, N.; Proserpio, D. M.; Sironi, A. Inorg. Chem. 1993, 32, 4829). In particular, the powder spectrum of the title compound shows the following: (i) the presence at low angles of broad, but well-defined, peaks (100 and 120) which are forbidden in Pmnm; (ii) a marked asymmetric broadening of some peaks (counterparted, in the "single-crystal" data collection, by anomalous peak widths of 1.8-2.0°); (iii) a structured background level. These features, which correspond to the streaks observed by Burrell on oscillation photographs, cannot be accounted for by ordinary twinning but are indicative of the paracrystalline and/or faulted nature of the crystals ( Guimer, A. X-ray Diffraction in Crystals, Imperfect Crystals and Amorphous Bodies; Freeman & Co.: San Francisco, CA, 1963. Reynolds, R. C. In Modern Powder Diffraction; Bish, D. L., Post, J. E., Eds.; Reviews in Mineralogy, 20.; The Mineralogical Society of America: Washington, DC, 1989; p 145). Consistently, we failed to satisfactory reproduce all such features by using, in a Rietveld refinement, any of the four structural models presented in the single-crystal analysis. However, some of these anomalies can be reproduced by our faulted model: (a) on nanocrystals, by the Debye interference function (Espinat, D.; Thevenot, F.; Grimound, J.; El Malki, K. J. Appl. Crystallogr. 1993, 26, 368) (b) on nanocrystals, by the explicit Fourier transform (Neder, R. B. Z. Kristallogr. 1994, Suppl. 8, 744); on infinitely thick crystals, by recursive algorithms (Treacy, M. M. J.; Newsam, J. M.; Deem, M. W. Proc. R. Soc. London, A 1991, 433, 499).
21. It is well-known that the simultaneous sampling of all reciprocal lattice nodes having the same 2θ makes the powder diffraction technique poorer (compared to standard single-crystal analysis), because severe (accidental or exact) overlaps of peaks occur. For the very same reason, however, (macro)twinning, i.e. the presence of two (or more) ordered macroscopic domains within each crystallite, does not affect the powder patterns, as long as preferred orientation of the crystallites is avoided (Li, J.; McCulley, F ; McDonnell, S. L.; Masciocchi, N.; Proserpio, D. M.; Sironi, A. Inorg. Chem. 1993, 32, 4829). In particular, the powder spectrum of the title compound shows the following: (i) the presence at low angles of broad, but well-defined, peaks (100 and 120) which are forbidden in Pmnm; (ii) a marked asymmetric broadening of some peaks (counterparted, in the "single-crystal" data collection, by anomalous peak widths of 1.8-2.0°); (iii) a structured background level. These features, which correspond to the streaks observed by Burrell on oscillation photographs, cannot be accounted for by ordinary twinning but are indicative of the paracrystalline and/or faulted nature of the crystals ( Guimer, A. X-ray Diffraction in Crystals, Imperfect Crystals and Amorphous Bodies; Freeman & Co.: San Francisco, CA, 1963. Reynolds, R. C. In Modern Powder Diffraction; Bish, D. L., Post, J. E., Eds.; Reviews in Mineralogy, 20.; The Mineralogical Society of America: Washington, DC, 1989; p 145). Consistently, we failed to satisfactory reproduce all such features by using, in a Rietveld refinement, any of the four structural models presented in the single-crystal analysis. However, some of these anomalies can be reproduced by our faulted model: (a) on nanocrystals, by the Debye interference function (Espinat, D.; Thevenot, F.; Grimound, J.; El Malki, K. J. Appl. Crystallogr. 1993, 26, 368) (b) on nanocrystals, by the explicit Fourier transform (Neder, R. B. Z. Kristallogr. 1994, Suppl. 8, 744); on infinitely thick crystals, by recursive algorithms (Treacy, M. M. J.; Newsam, J. M.; Deem, M. W. Proc. R. Soc. London, A 1991, 433, 499).
22. It is well-known that the simultaneous sampling of all reciprocal lattice nodes having the same 2θ makes the powder diffraction technique poorer (compared to standard single-crystal analysis), because severe (accidental or exact) overlaps of peaks occur. For the very same reason, however, (macro)twinning, i.e. the presence of two (or more) ordered macroscopic domains within each crystallite, does not affect the powder patterns, as long as preferred orientation of the crystallites is avoided (Li, J.; McCulley, F ; McDonnell, S. L.; Masciocchi, N.; Proserpio, D. M.; Sironi, A. Inorg. Chem. 1993, 32, 4829). In particular, the powder spectrum of the title compound shows the following: (i) the presence at low angles of broad, but well-defined, peaks (100 and 120) which are forbidden in Pmnm; (ii) a marked asymmetric broadening of some peaks (counterparted, in the "single-crystal" data collection, by anomalous peak widths of 1.8-2.0°); (iii) a structured background level. These features, which correspond to the streaks observed by Burrell on oscillation photographs, cannot be accounted for by ordinary twinning but are indicative of the paracrystalline and/or faulted nature of the crystals ( Guimer, A. X-ray Diffraction in Crystals, Imperfect Crystals and Amorphous Bodies; Freeman & Co.: San Francisco, CA, 1963. Reynolds, R. C. In Modern Powder Diffraction; Bish, D. L., Post, J. E., Eds.; Reviews in Mineralogy, 20.; The Mineralogical Society of America: Washington, DC, 1989; p 145). Consistently, we failed to satisfactory reproduce all such features by using, in a Rietveld refinement, any of the four structural models presented in the single-crystal analysis. However, some of these anomalies can be reproduced by our faulted model: (a) on nanocrystals, by the Debye interference function (Espinat, D.; Thevenot, F.; Grimound, J.; El Malki, K. J. Appl. Crystallogr. 1993, 26, 368) (b) on nanocrystals, by the explicit Fourier transform (Neder, R. B. Z. Kristallogr. 1994, Suppl. 8, 744); on infinitely thick crystals, by recursive algorithms (Treacy, M. M. J.; Newsam, J. M.; Deem, M. W. Proc. R. Soc. London, A 1991, 433, 499).
23. It is well-known that the simultaneous sampling of all reciprocal lattice nodes having the same 2θ makes the powder diffraction technique poorer (compared to standard single-crystal analysis), because severe (accidental or exact) overlaps of peaks occur. For the very same reason, however, (macro)twinning, i.e. the presence of two (or more) ordered macroscopic domains within each crystallite, does not affect the powder patterns, as long as preferred orientation of the crystallites is avoided (Li, J.; McCulley, F ; McDonnell, S. L.; Masciocchi, N.; Proserpio, D. M.; Sironi, A. Inorg. Chem. 1993, 32, 4829). In particular, the powder spectrum of the title compound shows the following: (i) the presence at low angles of broad, but well-defined, peaks (100 and 120) which are forbidden in Pmnm; (ii) a marked asymmetric broadening of some peaks (counterparted, in the "single-crystal" data collection, by anomalous peak widths of 1.8-2.0°); (iii) a structured background level. These features, which correspond to the streaks observed by Burrell on oscillation photographs, cannot be accounted for by ordinary twinning but are indicative of the paracrystalline and/or faulted nature of the crystals ( Guimer, A. X-ray Diffraction in Crystals, Imperfect Crystals and Amorphous Bodies; Freeman & Co.: San Francisco, CA, 1963. Reynolds, R. C. In Modern Powder Diffraction; Bish, D. L., Post, J. E., Eds.; Reviews in Mineralogy, 20.; The Mineralogical Society of America: Washington, DC, 1989; p 145). Consistently, we failed to satisfactory reproduce all such features by using, in a Rietveld refinement, any of the four structural models presented in the single-crystal analysis. However, some of these anomalies can be reproduced by our faulted model: (a) on nanocrystals, by the Debye interference function (Espinat, D.; Thevenot, F.; Grimound, J.; El Malki, K. J. Appl. Crystallogr. 1993, 26, 368) (b) on nanocrystals, by the explicit Fourier transform (Neder, R. B. Z. Kristallogr. 1994, Suppl. 8, 744); on infinitely thick crystals, by recursive algorithms (Treacy, M. M. J.; Newsam, J. M.; Deem, M. W. Proc. R. Soc. London, A 1991, 433, 499).
24. Thompson, J B., Jr. Am. Mineral. 1978, 63, 239. Niggli, A. Z. Kristallogr. 1959, 111, 288.
25. Thompson, J B., Jr. Am. Mineral. 1978, 63, 239. Niggli, A. Z. Kristallogr. 1959, 111, 288.
26. 1 for orthorhombic and monoclinic merging, respectively).
27. Biphasic crystals cannot be simulated by conventional single-crystal refinement programs.
28. A similar approach to polytypic macromolecular structures can be found in: Corradim, P.; Giunchi, C.; Petraccone, V.; Pirozzi, B.; Vidal, H. M. Gazz. Chim. Ital. 1980, 110, 413, and references therein.
29. Sirom, A.; Moret, M. To be submitted for publication.
30. Amouric, M.; Baronnet, A. Phys. Chem. Miner. 1983, 9, 146. Baronnet, A. In Minerals and Reactions at the Atomic Scale: Transmission Electron Microscopy, Buseck, P. R., Ed., Reviews in Mineralogy 27; The Mineralogical Society of America: Washington, DC, 1992; p 231.
31. Amouric, M.; Baronnet, A. Phys. Chem. Miner. 1983, 9, 146. Baronnet, A. In Minerals and Reactions at the Atomic Scale: Transmission Electron Microscopy, Buseck, P. R., Ed., Reviews in Mineralogy 27; The Mineralogical Society of America: Washington, DC, 1992; p 231.
32. Amelinckx, S. Acta Crystallogr. 1955, 8, 530; 1956, 9, 16; 1956, 9, 217.
33. Amelinckx, S. Acta Crystallogr. 1955, 8, 530; 1956, 9, 16; 1956, 9, 217.
34. Amelinckx, S. Acta Crystallogr. 1955, 8, 530; 1956, 9, 16; 1956, 9, 217.
35. Bruckner, S.; Meille, S. V.; Petraccone, V.; Pirozzi, B. Prog. Polym. Sci. 1991, 16, 361.
36. Zvyagin, B. B. Comput. Math. Appl. 1988, 16, 569.
37. Hikosaka, M.; Seto, T. Polym. J. 1973, 5, 111.