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Supplementary Material for Chemical Communications This journal is © The Royal Society of Chemistry 2003 SUPPLEMENTARY DATA A novel porous 3D network [Cu2(glutarate)4(4,4’-bipyridine)]·3H2O: Single-crystal-to-single-crystal reversible dehydration Beth Rather and Michael J. Zaworotko * Department of Chemistry, University of South Florida, 4202 E Fowler Ave (SCA 400), Tampa, FL, 33620, USA. Materials and Methods Thermogravimetric analysis was performed under nitrogen (except for the rehydration of 1a powder and crystals) on TA Instruments TGA 2950 Hi-Res. XRPD data were recorded on a Rigaku RU15 diffractometer at 30kV, 15mA for CuKα (λ = 1.5418 Å), with a scan speed of 1°/min and a step size of 0.02° in 2θ at room temperature. The simulated XRPD patterns were produced using Powder Cell for Windows Version 2.3. For guest readsorption experiments, the concentration changes were measured by GC using toluene as the internal standard. The data were fitted to the equation previously published by K. S. Min and M. P. Suh, Chem. Eur. J., 2001, 7, 303. Table of contents Figure S1. Conformational analysis of crystal structures containing the glutarate fragment and metals. Figure S2. FT-IR spectra of 1a and 1b. Figure S3. FT-IR spectra of compound 1b let in atmosphere for 55min (from t = 0 to t = 55min top to bottom). Figure S4. FT-IR spectra of compound 1b let in MeOH (HPLC grade H2O = 0.009%) for 1 night. Figure S5. FT-IR spectra of 2a, 2b and 2c. Figure S6. FT-IR spectra of 2a let in atmosphere for 45min (t=0 to t=45min from top to bottom) Figure S7. X-ray powder diffraction patterns of 1a (a) fresh sample, (b) calculated from the single crystal structure. Figure S8. X-ray powder diffraction patterns of 1b (a) sample heated to 150ºC, (b) calculated from the single crystal structure. Figure S9. X-ray powder diffraction patterns of 2a (a) fresh sample, (b) calculated from the single crystal structure. Figure S10. X-ray powder diffraction patterns of (a) blue powder formed during the synthesis of 1a and (b) simulation from the structure of [Co(4,4’- bipyridine)1.5(NO3)2]n (CSD code REJVUX). Figure S11. X-ray powder diffraction patterns of (a) blue crystals formed during the synthesis of 2a and (b) simulation from the structure of bilayer [Co(4,4’bipyridine)1.5(NO3)2]n (CSD code NAMSEZ). Figure S12. TGA trace of 1a. Figure S13. TGA traces of 1a (a) and 1b let in atmosphere for <1hour (b). Figure S14. TGA traces of the rehydration of 1b powder (a) and 1b crystals (b) under ambient atmosphere. Figure S15. TGA traces of 2a, 2b and 2c. Figure S16. Inclusion of apohost solid 1b with various guests from GC experiments. Supplementary Material for Chemical Communications This journal is © The Royal Society of Chemistry 2003 CSD Refcode C1-C4 MIYMOW 65 ZADJUJ 69 MEZSALa 69 XATNIPa 69.5 TODNAB 70 QANKOF 43 VIRYUQ 46 GLUECU 59 QIVHAE 62 MASXINa 62 ACBRUA 65 GLTECU 68 SIFWEJ 68 SUJXEA 68 HOTGOM 71 QIWKEM 71 TODNEF 74 QANKIZ disordered 60-66 OCENUF 166 MASXINb 169 XEDCUE 169 QIVGUX 172 TEGMIB 172 VIRZAX 173 CDGLTR 173 MIYMUC 175 FUMCUL 177 HOTHAZ 179 XATNIPb 179 MEZSALb 180 BOMXOQ Torsion Angles C2-C5 O1-C3 75 17.5 70 32 69 4.5 69.5 4 77 20 180 95 172 66.5 170 77.6 165 6 180 23 178 26.5 177 19.5 177 43.5 178 21.5 170 0.8 179 8 172 6.5 150-163 3-9 179 51 174 17 176 88 172 7 173 10 173 34.5 175 4.8 176 0.5 180 3.2 179 11 179 10 180 10 no structure O5-C3 43.5 82.5 4.5 4 7 35 85.4 31.5 77 70.5 87.5 27 54 48 75 49 49.5 30-77 34.5 21 88 7 15.5 95 0.35 32 0.3 8 10 10 Conformation Gauche-Gauche Gauche-Anti Anti-Anti Figure S1. Conformational analysis of crystal structures containing the glutarate fragment and metals. Compound 1a Compound 1b Figure S2. FT-IR spectra of 1a and 1b. Supplementary Material for Chemical Communications This journal is © The Royal Society of Chemistry 2003 Figure S3. FT-IR spectra of compound 1b let in atmosphere for 55min (from t = 0 to t = 55min top to bottom). Figure S4. FT-IR spectra of compound 1b let in MeOH (HPLC grade H2O = 0.009%) for 1 night. Compound 2a Compound 2b Supplementary Material for Chemical Communications This journal is © The Royal Society of Chemistry 2003 Compound 2c Figure S5. FT-IR spectra of 2a, 2b and 2c. Figure S6. FT-IR spectra of 2a let in atmosphere for 45min (t=0 to t=45min from top to bottom) a b Figure S7. X-ray powder diffraction patterns of 1a (a) fresh sample, (b) calculated from the single crystal structure. Supplementary Material for Chemical Communications This journal is © The Royal Society of Chemistry 2003 a b Figure S8. X-ray powder diffraction patterns of 1b (a) sample heated to 150ºC, (b) calculated from the single crystal structure. 5 10 15 19.52 20 25 25.30 30 36.89 37.36 32.95 36.54 37.05 33.46 33.97 34.43 34.89 35.31 35.83 32.57 31.39 31.96 30.69 29.61 30.10 28.84 28.15 27.31 26.62 29.24 24.10 24.59 25.92 16.31 22.32 22.68 23.13 23.20 21.67 20.57 19.98 18.43 0 16.66 14.61 15.41 25.01 12.8912.88 12.74 7.29 213 13.56 7.69 a er352 107 35 b Figure S9. X-ray powder diffraction patterns of 2a (a) fresh sample, (b) calculated from the single crystal structure. Supplementary Material for Chemical Communications This journal is © The Royal Society of Chemistry 2003 a 17.06 5 10 15 25 30 35.60 34.06 34.52 36.38 36.87 37.39 37.85 35.96 31.45 31.97 32.44 32.90 33.46 29.77 30.00 30.09 30.23 30.66 31.16 29.14 27.28 27.15 26.81 27.91 26.20 25.40 23.99 24.81 21.94 20 22.92 23.45 23.57 20.53 19.74 18.51 16.40 16.84 0 15.19 9.93 9.22 19.93 23.76 25.09 85 17.78 17.58 REJVUXEtOH 11.72 170 35 b Figure S10. X-ray powder diffraction patterns of (a) blue powder formed during the synthesis of 1a and (b) simulation from the structure of [Co(4,4’bipyridine)1.5(NO3)2]n (CSD code REJVUX). 8.88 5 10 17.49 13.84 15 20 25 30 35 37.32 37.94 38.24 38.82 39.34 37.07 36.46 35.76 34.89 35.15 34.25 37.50 30.09 30.35 30.67 31.20 31.45 31.88 32.36 32.85 33.36 26.46 25.13 23.06 26.84 27.58 28.13 28.68 29.27 26.03 25.43 23.22 23.77 24.33 21.72 20.39 17.24 25.01 20.82 21.42 16.72 11.55 14.71 13.53 11.82 10.67 26.2826.34 21.15 63 22.08 22.64 19.81 18.43 16.32 15.36 14.37 0 11.27 21.04 125 10.51 6.90 a NAMSEZ 40 b Figure S11. X-ray powder diffraction patterns of (a) blue crystals formed during the synthesis of 2a and (b) simulation from the structure of bilayer [Co(4,4’bipyridine)1.5(NO3)2]n (CSD code NAMSEZ). Supplementary Material for Chemical Communications This journal is © The Royal Society of Chemistry 2003 Figure S12. TGA trace of 1a. a b Figure S13. TGA traces of 1a (a) and 1b let in atmosphere for <1hour (b). Supplementary Material for Chemical Communications This journal is © The Royal Society of Chemistry 2003 a b Figure S14. TGA traces of the rehydration of 1b powder (a) and 1b crystals (b) under ambient atmosphere. a b Supplementary Material for Chemical Communications This journal is © The Royal Society of Chemistry 2003 c Figure S15. TGA traces of 2a, 2b and 2c. Guest G MeOH EtOH CH3CN n-hexane Guest (mol) included per unit formula of 1b 5.00.10-9 3.94.10-7 6.70.10-7 1.21.10-8 Figure S16. Inclusion of apohost solid 1b with various guests from GC experiments.