Study of Proton conductivity of a 2D flexible MOF and a 1D coordination polymer at higher temperature
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1 Supporting information Study of Proton conductivity of a 2D flexible MOF and a 1D coordination polymer at higher temperature Suresh Sanda, Soumava Biswas and Sanjit Konar* Department of Chemistry, IISER Bhopal, Bhopal , India. Fax: ; Tel: ; skonar@iiserb.ac.in Figure S1: Hydrogen bonding connectivity between the pyromellitate oxygen atoms and lattice water molecules (which are in between the layers) in compound 1. (Zn atoms and aldrithiol ligands are omitted for clarity). Colour code: C (grey), O (red).
2 Figure S2: Hydrogen bonding connectivity between pyromellitate oxygen atoms and lattice water molecules in compound 2. (Zn atoms and 4-pyridinethiolate ligands are omitted for clarity). Colour code: same as in fig. S1.
3 Figure S3: Hydrogen bonding network found in compound 1. Colour code: carbon (half grey), oxygen (red), nitrogen (blue), zinc (green). Sulphur (yellow). Hydrogen bonding connectivity (magenta). Figure S4: Hydrogen bonding network found in compound 2. Colour code: same as figure S3.
4 Figure S5: Water adsorption isotherm of compound 1. Figure S6: Water adsorption isotherm of compound 2.
5 Figure S7: PXRD patterns of compound 1. Simulated (black), Assynthesized (red). Table S1: Indexing result from the powder data of as-synthesized compound 1 collected at 25 deg From TREOR programme TRICLINIC P *** CONVENTIONAL CELL (METRIC SYMMETRY) * *** REDUCED-CELL *** A = ALFA = A = ALFA = B = BETA = B = BETA = C = GAMMA = C = GAMMA = VOLUME OF THE CONVENTIONAL CELL = A3 VOLUME OF THE REDUCED CELL = A3 H K L SST-OBS SST-CALC DELTA 2TH-OBS 2TH-CALC D-OBS FREE PARAM NUMBER OF OBS. LINES = 33 NUMBER OF CALC. LINES = 46
6 Figure S8: PXRD patterns of compound 2. Simulated (black), Assynthesized (red). Table S2: Indexing result from the powder data of as-synthesized compound 2 collected at 25 deg From TREOR programme TRICLINIC P *** CONVENTIONAL CELL (METRIC SYMMETRY) *** *** REDUCED-CELL *** A = ALFA = A = ALFA = B = BETA = B = BETA = C = GAMMA = C = GAMMA = VOLUME OF THE CONVENTIONAL CELL = A3 VOLUME OF THE REDUCED CELL = A3 H K L SST-OBS SST-CALC DELTA 2TH-OBS 2TH-CALC D-OBS FREE PARAM NUMBER OF OBS. LINES = 30 NUMBER OF CALC. LINES = 36
7 Figure S9: VT-PXRD of compound 1 in the range of C. Table S3: Indexing result from the powder data of as-synthesized compound 1 collected at 85 deg From TREOR programme TRICLINIC P *** CONVENTIONAL CELL (METRIC SYMMETRY) *** *** REDUCED-CELL *** A = ALFA = A = ALFA = B = BETA = B = BETA = C = GAMMA = C = GAMMA = VOLUME OF THE CONVENTIONAL CELL = A3 VOLUME OF THE REDUCED CELL = A3 H K L SST-OBS SST-CALC DELTA 2TH-OBS 2TH-CALC D-OBS FREE PARAM
8 NUMBER OF OBS. LINES = 32 NUMBER OF CALC. LINES = 47 Figure S10: VT-PXRD of compound 2 in the range of C. Table S4: Indexing result from the powder data of as-synthesized compound 2 collected at 85 deg From TREOR programme TRICLINIC P *** CONVENTIONAL CELL (METRIC SYMMETRY) *** *** REDUCED-CELL *** A = ALFA = A = ALFA = B = BETA = B = BETA = C = GAMMA = C = GAMMA = VOLUME OF THE CONVENTIONAL CELL = A3 VOLUME OF THE REDUCED CELL = A3 H K L SST-OBS SST-CALC DELTA 2TH-OBS 2TH-CALC D-OBS FREE PARAM NUMBER OF OBS. LINES = 22 NUMBER OF CALC. LINES = 38
9 Figure S11: PXRD patterns of as-synthesized (red) and humidified samples (at 80 C and 95% RH for 12 hours) of compound 1 (blue). Table S5: Indexing result from the powder data of humidified compound 1 at 80 deg, 95% RH. From TREOR programme TRICLINIC P *** CONVENTIONAL CELL (METRIC SYMMETRY) *** *** REDUCED-CELL *** A = ALFA = A = ALFA = B = BETA = B = BETA = C = GAMMA = C = GAMMA = VOLUME OF THE CONVENTIONAL CELL = A3 VOLUME OF THE REDUCED CELL = A3 H K L SST-OBS SST-CALC DELTA 2TH-OBS 2TH-CALC D-OBS FREE PARAM NUMBER OF OBS. LINES = 26 NUMBER OF CALC. LINES = 32
10 Figure S12: PXRD patterns of as-synthesized (red) and humidified samples (at 80 C and 95% RH for 12 hours) of compound 2 (blue). Table S6: Indexing result from the powder data of humidified compound 2 at 80 deg, 95% RH. From TREOR programme TRICLINIC P *** CONVENTIONAL CELL (METRIC SYMMETRY) *** *** REDUCED-CELL *** A = ALFA = A = ALFA = B = BETA = B = BETA = C = GAMMA = C = GAMMA = VOLUME OF THE CONVENTIONAL CELL = A3 VOLUME OF THE REDUCED CELL = A3 H K L SST-OBS SST-CALC DELTA 2TH-OBS 2TH-CALC D-OBS FREE PARAM NUMBER OF OBS. LINES = 23 NUMBER OF CALC. LINES = 26
11 Figure S13: DSC plot of compound 1 showing an endothermic peak at ~120 C correspond to phase change. Figure S14: DSC plot of compound 2 showing an endothermic peak at ~120 C correspond to phase change.
12 Figure S15: PXRD patterns of compound 1. As synthesized (red), After immersion in water for 24 hours (green). Table S7: Indexing result from the powder data of compound 1 immersed in H 2 O From TREOR programme TRICLINIC P *** CONVENTIONAL CELL (METRIC SYMMETRY) *** *** REDUCED-CELL *** A = ALFA = A = ALFA = B = BETA = B = BETA = C = GAMMA = C = GAMMA = VOLUME OF THE CONVENTIONAL CELL = A3 VOLUME OF THE REDUCED CELL = A3 H K L SST-OBS SST-CALC DELTA 2TH-OBS 2TH-CALC D-OBS FREE PARAM NUMBER OF OBS. LINES = 25 NUMBER OF CALC. LINES = 38
13 Figure S16: PXRD patterns of compound 2. As synthesized (red), After immersion in water for 24 hours (green). Table S8: Indexing result from the powder data of compound 2 immersed in H 2 O From TREOR programme TRICLINIC P *** CONVENTIONAL CELL (METRIC SYMMETRY) *** *** REDUCED-CELL *** A = ALFA = A = ALFA = B = BETA = B = BETA = C = GAMMA = C = GAMMA = VOLUME OF THE CONVENTIONAL CELL= A3 VOLUME OF THE REDUCED CELL= A3 H K L SST-OBS SST-CALC DELTA 2TH-OBS 2TH-CALC D-OBS FREE PARAM NUMBER OF OBS. LINES = 31 NUMBER OF CALC. LINES = 33
14 Figure S17: Nyquist plots of compound 1 at 25 C, 30 C, 35 C and 95% RH. (For 303 K and 308 K the error bars are contained within the plot-shape) Figure S18: Nyquist plots of compound 1 at 76 C, 78 C, 80 C and 95% RH. (Error bars are contained within the plot-shape)
15 Figure S19: Nyquist plots of compound 2 at 25 C, 30 C, 35 C and 95% RH. Figure S20: Nyquist plots of compound 2 at 76 C, 78 C, 80 C and 95% RH.
16 Figure S21: TGA plots as-synthesized (black) and humidified (at 80 C and 95% RH) samples (red) of compound 1. Figure S22: TGA plots as-synthesized (black) and humidified (at 80 C and 95% RH) samples (red) of compound 2.
17 Figure S23: TGA plots as-synthesized (black) and dehydrated samples (green) of compound 1. Figure S24: TGA plots as-synthesized (black) and dehydrated samples (green) of compound 2.
18 Figure S25: IR spectrum of compound 1. D 2 O. (Broad peak at 2500 cm -1 which is due to O-D stretching frequency and confirms the D 2 O exchange) Figure S26: IR spectrum of compound 2. D 2 O. (Broad peak at 2500 cm -1 which is due to O-D stretching frequency and confirms the D 2 O exchange)
19 Figure S27: Nyquist plot of compound 1.D 2 O at 80 C, 95% RH. Figure S28: Nyquist plot of compound 2.D 2 O at 80 C, 95% RH.
20 Figure S29: Plausible water molecule accumulation inside the framework of compound 1. (Calculated through Monte Carlo simulations from Material Studio 6.1 program using sorption module) Figure S30: A view of water density distribution inside the framework of compound 1 (Calculated through Monte Carlo simulations from Material Studio 6.1 program using sorption module). (Bonding connectivity between the framework atoms is removed for clarity).
21 Figure S31: Plausible water accumulation inside the framework of compound 2. (Calculated through Monte Carlo simulations from Material Studio 6.1 program using sorption module). Figure S32: A view of water density distribution inside the framework of compound 2 (Calculated through Monte Carlo simulations from Material Studio 6.1 program using sorption module). (Bonding connectivity between the framework atoms is removed for clarity).
22 Figure S33: Nyquist plots of compound 1 at 25 C and 75%, 85%, 95% RH. Figure S34: Nyquist plots of compound 2 at 25 C and 75%, 85%, 95% RH.
23 Figure S35: Nyquist plot of dehydrated compound 1 at 25 C and 95% RH. Figure S36: Nyquist plot of dehydrated compound 2 at 25 C and 95% RH.
24 Figure S37: Relative humidity vs conductivity plot of dehydrated compound 1 at 25 C, adsorption isotherm of compound 1 in the range of P/P 0 = 0.4 to 1 bar (inset). Figure S38: Relative humidity vs conductivity plot of dehydrated compound 2 at 25 C, adsorption isotherm of compound 2 in the range of P/P 0 = 0.4 to 1 bar (inset).
25 Figure S39: Nyquist plots of compound 1 at 35%, 45% RH and 80 C. Figure S40: Nyquist plots of compound 1 at 85%, 95% RH and 80 C.
26 Figure S41: Nyquist plots of compound 2 at 35%, 45% RH and 80 C. Figure S42: Nyquist plots of compound 2 at 85%, 95% RH and 80 C.
27 Figure S43: Relative humidity vs conductivity plot of compound 1 at 80 C. Figure S44: Relative humidity vs conductivity plot of compound 2 at 80 C.
28 Figure S45: Nyquist plots of compound 1 at 25 C, 35 C and zero humidity. Figure S46: Nyquist plots of compound 1 at 75 C, 80 C and zero humidity.
29 Figure S47: Conductivity vs temperature plot of compound 1 under anhydrous conditions. Figure S48: The time-dependent proton conductivity experiments of compounds 1 in 3 different cycles at 80 C, 95% RH.
30 Figure S49: The time-dependent proton conductivity experiments of compounds 1 in 3 cycles at 80 C, 95% RH. Figure S50: PXRD patterns of compound 1. As synthesized sample (black), after time dependent conductivity measurement for 10 hours (pink).
31 Figure S51: PXRD patterns of compound 2. As synthesized sample (black), after time dependent conductivity measurement for 10 hours (pink).
Supporting Information
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