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0345666843
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note
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4F (23 mg, 0.6 mmol)-if desired- and 1,3,5-mmethylbenzene (TMB, 2.0 g, 17 mmol) were added. After at least 45 min at 35-40 °C, tetraethoxysilane (4.4 g, 21 mmol) was added. After 20 h at 35-40 °C, the cloudy mixture was kept at 95-100 (samples P- - -) or 120 °C (samples Z- - -) for 24 h. The filtered precipitate was dried in air (4.9 g of white, as-made silica). Typical yields: 94-100% based on Si. As-made silicas were calcined at 500 °C for 8 h in air to yield MCFs.
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9
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0027807060
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X-ray powder diffraction (XRD) patterns were recorded on a Scintag PADX diffractometer using Cu Kα radiation detected by a Si(Li) solid-state detector cooled by a Peltier cell. The data were desmeared by the direct method: Singh, M. A.; Ghosh, S. S.; Shannon, R. F. J. Appl. Crystallogr. 1993, 26, 787.
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0015506135
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d, and was weighted to lie on desmeared data for 2θ > 2° and on local minima of the desmeared data for 2θ < 2°. See: Mateu, L.; Tardieu, A.; Luzzati, V.; Aggerbeck, L.; Scanu, A. M. J. Mol. Biol. 1972, 70, 105.
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0344803996
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note
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Transmission electron microscopy was performed on a JEOL 2000 microscope (200 kV) using copper grids.
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13
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0344372146
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note
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(a) Nitrogen sorption was carried out on a Micromeritics ASAP 2000 system at 77 K with samples outgassed at 180-200 °C under high vacuum for at least 4 h.
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18
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0344803992
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note
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Full-width-at-half-maximum (fwhm) values (Table 1) depend on the number of data points, equilibration time, etc., so they represent upper limits. We expect the actual size distributions to be smaller, which is in agreement with X-ray simulation experiments (see text).
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20
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After review of this paper, a related mechanism was described for surface-templated inverse opal structures. See: Zakhidov, A. A.; Baughman, R. H.; Iqbal, Z.; Cui, C.; Khayrullin, I.; Dantas, S. O.; Marti, J.; Ralchenko, V. G. Science 1998, 282, 897.
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