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1 Supporting Information A Co-Ca Phosphonate Showing Humidity Sensitive Single Crystal-to-Single Crystal Structural Transformation and Tunable Proton Conduction Properties Song-Song Bao, Nan-Zhu Li, Jared M. Taylor, Yang Shen, Hiroshi Kitagawa, Li-Min Zheng, * State Key Laboratory of Coordination Chemistry, School of Chemistry and Chemical Engineering, Collaborative Innovation Center of Advanced Microstructures, Nanjing University, Nanjing , P. R. China Division of Chemistry, Graduate School of Science, Kyoto University, Kitashirakawa-Oiwakecho, Sakyo-ku, Kyoto , Japan S1
2 Table S1 Selected bond lengths (Å) and angles ( ) for CoCa 4H 2 O and CoCa 2H 2 O (296 K). CoCa 4H 2 O CoCa 2H 2 O CoCa 4H 2 O CoCa 2H 2 O Co(1)-O(1) 1.942(3) 1.942(5) Ca(1)-O(9C) 2.309(3) 2.308(5) Co(1)-O(4) 1.934(3) 1.938(6) P(1)-O(1) 1.537(3) 1.538(5) Co(1)-O(7) 1.917(3) 1.912(5) P(1)-O(2) 1.479(3) 1.476(6) Co(1)-N(1) 1.949(3) 1.944(6) P(1)-O(3) 1.561(3) 1.566(6) Co(1)-N(2) 1.940(3) 1.944(6) P(2)-O(4) 1.524(3) 1.538(6) Co(1)-N(3) 1.938(4) 1.938(7) P(2)-O(5) 1.489(3) 1.488(6) Ca(1)-O(1W) 2.429(4) 2.408(6) P(2)-O(6) 1.562(3) 1.560(6) Ca(1)-O(2W) (3) 2.480(6) P(3)-O(7) 1.539(3) 1.546(6) Ca(1)-O(5) 2.298(3) 2.279(6) P(3)-O(8) 1.515(3) 1.506(6) Ca(1)-O(2A) 2.273(3) 2.286(6) P(3)-O(9) 1.520(3) 1.526(4) Ca(1)-O(8B) 2.316(6) 2.337(6) O(1)-Co(1)-O(4) 90.37(13) 90.3(2) O(1W)-Ca(1)-O(2W) 79.75(12) 80.47(19) O(1)-Co(1)-O(7) 89.79(12) 90.6(2) O(1W)-Ca(1)-O(5) 92.70(12) 93.5(2) O(1)-Co(1)-N(1) 89.13(13) 89.3(2) O(1W)-Ca(1)-O(2A) 90.53(12) 90.58(19) O(1)-Co(1)-N(2) (14) 177.4(2) O(1W)-Ca(1)-O(8B) 87.56(11) 85.84(19) O(1)-Co(1)-N(3) 91.83(14) 91.3(2) O(1W)-Ca(1)-O(9C) (12) 165.8(2) O(4)-Co(1)-O(7) 90.46(12) 89.6(2) O(2W)-Ca(1)-O(5) (11) (19) O(4)-Co(1)-N(1) 91.58(15) 92.2(3) O(2W)-Ca(1)-O(2A) 85.68(11) 86.86(19) O(4)-Co(1)-N(2) 89.34(15) 89.9(3) O(2W)-Ca(1)-O(8B) 90.28(11) 92.46(19) O(4)-Co(1)-N(3) (14) 178.3(2) O(2W)-Ca(1)-O(9C) 87.16(11) 85.29(19) O(7)-Co(1)-N(1) (16) 178.2(3) O(5)-Ca(1)-O(2A) 90.09(11) 90.2(2) O(7)-Co(1)-N(2) 92.70(13) 92.1(2) O(5)-La(1)-O(8B) 93.75(11) 90.1(2) O(7)-Co(1)-N(3) 89.51(14) 89.5(2) O(5)-La(1)-O(9C) (11) 100.7(2) N(1)-Co(1)-N(2) 88.40(14) 88.1(2) O(2A)-La(1)-O(8B) (11) 176.4(2) N(1)-Co(1)-N(3) 88.49(16) 88.7(3) O(2A)-La(1)-O(9C) 89.32(11) 88.73(19) N(2)-Co(1)-N(3) 88.46(16) 88.7(3) O(8B)-La(1)-O(9C) 91.68(11) 94.72(19) Symmetry transformations used to generate equivalent atoms: For CoCa 4H 2 O, A: 3/2-x, 1/2+y, 3/2-z; B: -1/2+x, 1/2-y, -1/2+z; C: 3/2-x, -1/2+y, 3/2-z. For CoCa 2H 2 O, A: 1/2-x, 1/2+y, 1/2-z; B: -1/2+x, 3/2-y, -1/2+z; C: 1/2-x, -1/2+y, 1/2-z. S2
3 Table S2 Selected bond lengths (Å) and angles ( ) for CoCa 4H 2 O at 296 K and 123 K. 296 K 123 K 296 K 123 K Co(1)-O(1) 1.942(3) 1.935(3) Ca(1)-O(9C) 2.309(3) 2.305(3) Co(1)-O(4) 1.934(3) 1.931(3) P(1)-O(1) 1.537(3) 1.529(3) Co(1)-O(7) 1.917(3) 1.919(3) P(1)-O(2) 1.479(3) 1.477(3) Co(1)-N(1) 1.949(3) 1.946(4) P(1)-O(3) 1.561(3) 1.559(3) Co(1)-N(2) 1.940(3) 1.941(4) P(2)-O(4) 1.524(3) 1.527(3) Co(1)-N(3) 1.938(4) 1.941(4) P(2)-O(5) 1.489(3) 1.490(3) Ca(1)-O(1W) 2.429(4) 2.423(3) P(2)-O(6) 1.562(3) 1.565(3) Ca(1)-O(2W) (3) 2.475(3) P(3)-O(7) 1.539(3) 1.532(3) Ca(1)-O(5) 2.298(3) 2.287(3) P(3)-O(8) 1.515(3) 1.506(3) Ca(1)-O(2A) 2.273(3) 2.270(3) P(3)-O(9) 1.520(3) 1.516(3) Ca(1)-O(8B) 2.316(6) 2.315(3) O(1)-Co(1)-O(4) 90.37(13) 90.00(13) O(1W)-Ca(1)-O(2W) 79.75(12) 80.14(12) O(1)-Co(1)-O(7) 89.79(12) 90.02(13) O(1W)-Ca(1)-O(5) 92.70(12) 92.01(13) O(1)-Co(1)-N(1) 89.13(13) 89.32(15) O(1W)-Ca(1)-O(2A) 90.53(12) 91.98(13) O(1)-Co(1)-N(2) (14) (15) O(1W)-Ca(1)-O(8B) 87.56(11) 88.28(12) O(1)-Co(1)-N(3) 91.83(14) 91.81(15) O(1W)-Ca(1)-O(9C) (12) (13) O(4)-Co(1)-O(7) 90.46(12) 90.50(13) O(2W)-Ca(1)-O(5) (11) (11) O(4)-Co(1)-N(1) 91.58(15) 91.82(16) O(2W)-Ca(1)-O(2A) 85.68(11) 86.38(11) O(4)-Co(1)-N(2) 89.34(15) 89.53(16) O(2W)-Ca(1)-O(8B) 90.28(11) 90.24(11) O(4)-Co(1)-N(3) (14) (15) O(2W)-Ca(1)-O(9C) 87.16(11) 87.02(11) O(7)-Co(1)-N(1) (16) (16) O(5)-Ca(1)-O(2A) 90.09(11) 90.19(12) O(7)-Co(1)-N(2) 92.70(13) 92.25(15) O(5)-La(1)-O(8B) 93.75(11) 93.28(12) O(7)-Co(1)-N(3) 89.51(14) 89.48(15) O(5)-La(1)-O(9C) (11) (11) N(1)-Co(1)-N(2) 88.40(14) 88.44(16) O(2A)-La(1)-O(8B) (11) (12) N(1)-Co(1)-N(3) 88.49(16) 88.22(17) O(2A)-La(1)-O(9C) 89.32(11) 87.68(11) N(2)-Co(1)-N(3) 88.46(16) 88.66(17) O(8B)-La(1)-O(9C) 91.68(11) 91.29(11) Symmetry transformations used to generate equivalent atoms: A: 3/2-x, 1/2+y, 3/2-z; B: -1/2+x, 1/2-y, -1/2+z; C: 3/2-x, -1/2+y, 3/2-z. S3
4 - Table S3 Hydrogen bonds among phosphonate, water molecules and ClO 4 CoCa 4H 2 O (123 K). anions in D-H A d(d-h) (Å) d(h A) (Å) d(d A) (Å) DHA ( ) O1W-H1WA O2W i (4) 167 O1W-H1WB O1 ii (5) 164 O2W-H2WA O4W i (5) 159 O2W-H2WB O7 ii (4) 130 O3W-H3WA O5W v (4) 153 O3W-H3WB O9 iii (5) 172 O4W-H4WA O5W v (4) 174 O4W-H4WB O8 iii (5) 152 O5W-H5WA O10 vi (5) 170 O5W-H5WB O (7) 157 O6W-H6WA O10 vii (5) 111 O6W-H6WB O12 viii (6) 117 O3-H3C O3W iv (4) 177 O6-H6C O4w ix (5) 165 Symmetry transformations used to generate equivalent atoms: i: 1-x, 1-y, 1-z; ii: -1/2+x, 1/2-y,-1/2+z; iii: -3/2+x, 1/2-y, -3/2+z; iv: -1/2+x, -1/2-y, -1/2+z; v: 3/2-x, 1/2+y, 1/2-z; vi: 1-x, 1-y, -z; vii: 1/2-x, -1/2+y, 1/2-z; viii: -1/2+x, 3/2-y, 1/2+z; ix: 3/2-x, -1/2+y, 3/2-z. - Table S4 Hydrogen bonds among phosphonate, water molecules and ClO 4 CoCa 4H 2 O (296 K). anions in D-H A d(d-h) (Å) d(h A) (Å) d(d A) (Å) DHA ( ) O1W-H1WA O2W i (4) 167 O1W-H1WB O1 ii (4) 164 O2W-H2WA O4W i (5) 159 O2W-H2WB O7 ii (4) 130 O3W-H3WA O5W v (4) 150 O3W-H3WB O9 iii (5) 172 O4W-H4WA O5W v (4) 171 O4W-H4WB O8 iii (5) 152 O5W-H5WA O10 vi (5) 171 O5W-H5WB O (5) 154 O6W-H6WA O10 vii (5) 115 O6W-H6WB O12 viii (4) 114 O3-H3C O3W iv (4) 173 O6-H6C O4w ix (4) 162 Symmetry transformations used to generate equivalent atoms: i: 1-x, 1-y, 1-z; ii: -1/2+x, 1/2-y,-1/2+z; iii: -3/2+x, 1/2-y, -3/2+z; iv: -1/2+x, -1/2-y, -1/2+z; v: 3/2-x, 1/2+y, 1/2-z; vi: 1-x, 1-y, -z; vii: 1/2-x, -1/2+y, 1/2-z; viii: -1/2+x, 3/2-y, 1/2+z; ix: 3/2-x, -1/2+y, 3/2-z. S4
5 - Table S5 Hydrogen bonds among phosphonate, water molecules and ClO 4 CoCa 2H 2 O (296 K). anions in D-H A d(d-h) (Å) d(h A) (Å) d(d A) (Å) DHA ( ) O1W-H1WA O2W i (7) 156 O1W-H1WB O1 ii (6) 167 O2W-H2WB O4W iii (8) 158 O2W-H2WA O7 ii (7) 117 O3W-H3WA O9 iv (8) 174 O3W-H3WB O12 v (7) 132 O4W-H4WA O (8) 171 O4W-H4WB O8 ii (7) 163 O3-H3C O3W (8) 172 O6-H6C O4w vi (8) 159 Symmetry transformations used to generate equivalent atoms: i: -x, 2-y, -z; ii: -1/2+x, 3/2-y, -1/2+z; iii: -x, 1-y, -z; iv: x, -1+y, z; v: 3/2+x, 3/2-y, 3/2+z; vi: 1/2-x, 1/2+y, 1/2-z. S5
6 CoCa 4H 2 O CoCa 2H 2 O wavelength (cm -1 ) Figure S1. IR spectra of CoCa 2H 2 O and CoCa 4H 2 O. Counts 2,600 2,400 2,200 2,000 1,800 1,600 1,400 1,200 1, hkl_phase 0.00 % Th (Degree) Figure S2. Pawley fit of the fully dehydrated sample of CoCa nh 2 O under vacuum performed using Topas 4.2 program. Cell parameters: P2 1 /n, a = Å, b = Å, c = Å, β = , V = Å 3. (Rwp = 4.96). S6
7 CoCa 4H 2 O-simulated (e) CoCa 4H 2 O-exptl. (d) (c) CoCa 2H 2 O-exptl. (b) CoCa 2H 2 O-simulated (a) θ ( ο ) Figure S3. The PXRD patterns of (a) CoCa 2H 2 O simulated from single-crystal X-ray diffraction result; (b) powder samples of CoCa 2H 2 O; (c) the resulting sample after water adsorption and desorption measurements; (d) powder samples of CoCa 4H 2 O and (e) CoCa 4H 2 O simulated from single-crystal X-ray diffraction result. S7
8 (a) (b) Figure S4. Differential heat of adsorption (a) and desorption (b) of CoCa nh 2 O, determined from H 2 O adsorption isotherms at 15 o C, 25 o C and 35 o C, respectively. The average heat of adsorption in water coverage range is 50.8 kj mol -1. The average heat of desorption in water coverage range is 58.0 kj mol -1. S8
9 Figure S5. Nyquist plots for the pellet of CoCa nh 2 O at 298 K and various RH. Up: RH increases from 40 to 95%; Middle: The enlarged view of graph; Bottom: The enlarged view of the Nyquist plot measured at 298 K and 95% RH. S9
10 Figure S6. Nyquist plots for the pellet of CoCa nh 2 O at 298 K and RH decreases from 95 to 60%. Figure S7. Nyquist plots for the pellet of CoCa nh 2 O at 90% RH and various temperatures. S10
11 Figure S8. Crystal faces (001), (102) and (10-1) of CoCa nh 2 O were determined. Figure S9. A single crystal of CoCa nh 2 O was cut into rectangle to expose the crystal face (010) for ac impedance measurement along [010] direction. Figure S10. Nyquist plots for single crystal sample of CoCa nh 2 O along [010] at 298 K and RH increases from 55 to 95%. S11
12 Figure S11. Nyquist plots for single crystal sample of CoCa nh 2 O along [010] at 298 K and RH decreases from 95 to 50%. Figure S12. Nyquist plots for single crystal sample of CoCa nh 2 O along [202] at 298 K and RH increases from 55 to 95%. S12
13 Figure S13. Nyquist plots for single crystal sample of CoCa nh 2 O along [202] at 298 K and RH decreases from 95 to 50%. Figure S14. Nyquist plots for single crystal sample of CoCa nh 2 O along [20-1] at 298 K and RH increases from 55 to 95%. S13
14 Figure S15. Nyquist plots for single crystal sample of CoCa nh 2 O along [20-1] at 298 K and RH decreases from 95 to 55%. Figure S16. The proposed proton conduction pathway along the [010] direction. S14
15 Figure S17. Nyquist plots for single crystal sample of CoCa nh 2 O along [010] at 90% RH and various temperatures. Figure S18. Nyquist plots for single crystal sample of CoCa nh 2 O along [202] at 90% RH and various temperatures. S15
16 Figure S19. Nyquist plots for single crystal sample of CoCa nh 2 O along [20-1] at 90% RH and various temperatures. Figure S20. Plots of log(σt) vs 1000/T for bulk and single crystal sample of CoCa nh 2 O at 90% relative humidity. The solid lines represent the best fits of the data. S16
17 Figure S21. Impedance response to the relative humidity at different frequencies for single crystal sample of CoCa nh 2 O along [010] direction ( mm 3 ). Figure S22. Impedance response and recovery time to RH variation between 55 % and 95 % for powder samples of CoCa nh 2 O measured at 1 khz and 0.1 V. S17
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