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SUPPLEMENTARY MATERIAL
Water vapour uptake and extrusion by a crystalline metallorganic solid based on half-sandwich Ru(II) building-blocks
Alessia Bacchi,*a Giulia Cantoni,a Michele R. Chierotti,b Alberto Girlando,a Roberto Gobetto,b Giuseppe Lapadula,c Paolo Pelagatti,*a Angelo Sironi,c and Matteo Zecchinia
a Dipartimento di Chimica GIAF, University of Parma, Viale G.P. Usberti 17/A, 43124 Parma, Italy. Fax: +390521905557; Tel: +390521905421; E-mail: [email protected]; [email protected] (Tel. +390521905426) b Dipartimento di Chimica I.F.M., University of Turin, Via P. Giuria 7, 10125 Turin, Italy. Fax: +390116707881; Tel: +390116707523; E-mail: [email protected] cDipartimento di Chimica Strutturale e Stereochimica Inorganica, University of Milan, via Venezian 21, 20133 Milan, Italy. Fax: +390250314454; Tel: +390250314440; Email: [email protected]
Supplementary Material (ESI) for CrystEngCommThis journal is (c) The Royal Society of Chemistry 2011
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659.
4469
7.43
772.
8478
9.37
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0285
4.221055
.07
1088
.93
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1197
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1224
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1236
.61
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Figure SI1 ATR-FTIR spectrum of 1α
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8.60
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7.98
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679.
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1880
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.71
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.25
1158
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1199
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1211
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1228
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.57
1328
.49
1387
.71
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1618
.77
1709
.36
2497
.08
2960
.33
3343
.32
3493
.78
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%R
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500 1000 1500 2000 2500 3000 3500 4000 Wavenumbers (cm-1)
Figure SI2 ATR-FTIR spectrum of wet
Supplementary Material (ESI) for CrystEngCommThis journal is (c) The Royal Society of Chemistry 2011
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%R
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500 1000 1500 2000 2500 3000 3500 4000 Wavenumbers (cm-1)
Figure SI3 ATR-FTIR spectrum of wet (black) after thermal treatment at 90°C under vacuum (red) (partial exposure to air moisture).
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Figure SI4 TGA analysis of wet (1st run)
Figure SI5 TGA analysis of wet (2nd run); the sample of the 1st run has been cooled in air and subjected to a second TGA analysis
1st run obs. weight loss: 4.29% calc. weight loss: 4.03%
1st run obs. weight loss: 4.04% calc. weight loss: 4.03%
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Figure SI6 Comparison of the XRPD spectra of wet calculated (red) and obtained after exposure of 1α to water vapour (black).
Figure SI7 Final Rietveld refinement for 1β the high angle region has been magnified (4X) for clarity of the plot.
wet - experimental calculated
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Figure SI8. 1H–13C FSLG-HETCOR spectrum of 1α recorded with a spinning speed of 12 kHz and a contact time of 100 µs.
Figure SI9. 1H–13C FSLG-HETCOR spectrum of wet recorded with a spinning speed of 12 kHz and a contact time of 100 µs.
Supplementary Material (ESI) for CrystEngCommThis journal is (c) The Royal Society of Chemistry 2011
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Figure SI10. 1H–13C FSLG-HETCOR spectrum of 1β recorded with a spinning speed of 12 kHz and a contact time of 100 µs.
Figure SI11. 13C CPMAS spectra of compounds INA (a), A4AB (b) and [(p-cymene)Ru(κN-A4AB)Cl2] (c) recorded at 100.65 MHz with a spinning speed of 12 kHz.
Supplementary Material (ESI) for CrystEngCommThis journal is (c) The Royal Society of Chemistry 2011
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Figure SI12. 1H MAS spectra of compounds α (a), wet (b) and β (c) recorded at 400.23 MHz with a spinning speed of 32 kHz.
a)
b)
c)
Scheme SI1. Hydrogen bond arrangements in INA (a), A4AB (b) and [(p-cymene)Ru(κN-A4AB)Cl2] (c).
Supplementary Material (ESI) for CrystEngCommThis journal is (c) The Royal Society of Chemistry 2011
