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34547952007
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Synthesis of (1, An amount of 0.0408 g (0.125 mmol) of In 2S3, 0.051 g (0.15 mmol) of Sb2S3, and 0.016 g (0.5 mmol) of S were combined and loaded in a 3/8 inch Pyrex tube along with 0.30 mL of 1:1 dipropylamine:water in air. The tube was then evacuated to <3 × 10-3 Torr and flame-sealed. The tube was kept in an oven at ∼160 °C for 5 days. The products were isolated in air by filtration and washed with deionized water, ethanol, and ether. The product consists of pale yellow platelike crystals along with some recrystallized Sb2S3 (20, Yield was ∼60, The crystals appear to be stable in air for months. Energy-dispersive spectroscopy (EDS) results: In 4.98Sb6S18.96. C, H, N analysis, 14.74, 3.48, 2.87 caled: 14.70, 3.38, 2.86
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18.96. C, H, N analysis (%); 14.74, 3.48, 2.87 (caled: 14.70, 3.38, 2.86).
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31
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34547955875
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Compound (1) crystal data: The single-crystal X-ray diffraction data was collected with a STOE IPDS diffractometer at 100 K. A platelike crystal with dimensions 0.178 × 0.245 × 0.042 mm3 was chosen for data collection. An analytical absorption correction based on face-indexing was applied. The structure was solved with direct methods using SHELX-97. The PLATON SQUEEZE program was applied to obtain better refinement for the highly disordered organic cations and water molecule. Space group: P2/c with a, 17.638(4) Å, b, 9.4889-(19) Å, c, 26.369(5) Å, b, 115.47(3)°, V, 3984.2(14) Å3. Other crystal data: Z, 2, Dcaled, 2.041 g cm-3, m, 3.942 mm -1; index range -22 ≤ h ≤ 20, 12 ≤ k ≤ 12, 32 ≤ l ≤ 31; total reflections 29779, independent reflections 8185, parameters 228, R1, 5.84, wR2, 15.47, GOF, 1.096
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-1; index range -22 ≤ h ≤ 20. -12 ≤ k ≤ 12. -32 ≤ l ≤ 31; total reflections 29779, independent reflections 8185, parameters 228, R1 = 5.84 %, wR2 = 15.47 %, GOF = 1.096.
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33
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0000054071
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Estermann, M.; McCusker, L. B.; Baerlocher, C.; Merrouche, A.; Kessler, H. Nature 1991, 352, 320.
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35
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34547928678
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19 (91% exchange yield).
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19 (91% exchange yield).
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36
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33745959378
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Manos, M. J.; Chrissafis, K.; Kanatzidis, M. G. J. Am. Chem. Soc. 2006, 128, 8875.
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0000099977
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+-exchange capacity was reported by Behrens, E. A.; Poojary, D. M.; Clearfield, A. Chem. Mater. 1996, 8, 1236.
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+-exchange capacity was reported by Behrens, E. A.; Poojary, D. M.; Clearfield, A. Chem. Mater. 1996, 8, 1236.
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38
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34547961853
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Single-crystal diffraction data was collected at 100 K, and powder XRD was obtained at room temperature; therefore, there is a slight shift to lower 2θ (∼ .32 Å in d-spacing fo the (010) reflection) in the experimental PXRD pattern compared to the calculated one.
-
(a) Single-crystal diffraction data was collected at 100 K, and powder XRD was obtained at room temperature; therefore, there is a slight shift to lower 2θ (∼ .32 Å in d-spacing fo the (010) reflection) in the experimental PXRD pattern compared to the calculated one.
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39
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34547951449
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3. However, because of the deteriorated quality of the ion-exchanged single crystal, the refinement of the structure is not satisfactory. Nevertheless, the framework connectivity could be confirmed to be the same as the pristine material.
-
3. However, because of the deteriorated quality of the ion-exchanged single crystal, the refinement of the structure is not satisfactory. Nevertheless, the framework connectivity could be confirmed to be the same as the pristine material.
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40
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34547962595
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19 was then added in the salt solutions. The mixture was kept at 75 °C without stirring for ∼24 h. The products were isolated in air by filtration and washed with water, ethanol, and ether. The crystallinity of the sample was confirmed by X-ray diffraction before and after ion-exchange.
-
19 was then added in the salt solutions. The mixture was kept at 75 °C without stirring for ∼24 h. The products were isolated in air by filtration and washed with water, ethanol, and ether. The crystallinity of the sample was confirmed by X-ray diffraction before and after ion-exchange.
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41
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34547929714
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Ding, N.; Kanatzidis, M. G. unpublished results.
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Ding, N.; Kanatzidis, M. G. unpublished results.
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42
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34547943997
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