Effects of Water on the Forward and Backward Conversions of Lead(II) Iodide to Methylammonium Lead Perovskite
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1 Eletroni Supplementary Material (ESI) for Journal of Materials Chemistry A. This journal is The Royal Soiety of Chemistry 2017 Supporting Information Effets of Water on the Forward and Bakward Conversions of Lead(II) Iodide to Methylammonium Lead Perovskite Kazutaka Shoyama, a Wataru Sato, a Yunlong Guo, a,b * and Eiihi Nakamura a * a. Department of Chemistry, The University of Tokyo Hongo, Bunkyo-ku, Tokyo , Japan. *nakamura@hem.s.u-tokyo.a.jp; guoyunlong@ias.a.n. b. Beijing National Laboratory for Moleular Sienes, Institute of Chemistry, Chinese Aademy of Sienes, Beijing , P. R. China. * guoyunlong@ias.a.n. 1
2 X-ray diffration data Figure S1. 1-D traes of XRD experiment. a, Referene alulated XRD patterns of PI 1, INT- W 2, TA 3, and PVK (at 20 C and 127 C) 4. b, XRD pattern of a rystal obtained by mixing of MAI and PI in water., XRD patterns of fiber XRD measurement. Crystallographi analysis The diffration images for X-ray rystallographi analysis were olleted on a Rigaku Rapid II diffratometer equipped with an imaging plate (IP) using Cu Kα (λ = Å) radiation. For rystallographi analysis, the sample was removed from the mother liquor and put onto a glass slide. A rystal was hosen and then it was put on and taken off from a glass slide several times to remove liquid from its surfae. The positional and thermal parameters were refined by the full-matrix least-squares method using SHELXL-2014/7 program. The Yadokari-XG software was used for refinement of the struture. 2
3 Crystallographi data of INT-W ( 150 C) Formula I 3 Pb, CH 6 N, O Formula weight Measurement temperature 123(2) K Crystal system monolini Spae group P2 1 /m Lattie parameters a = (4) Å b = (2) Å = (5) Å α = 90 β = (7) γ = 90 Volume (4) Å 3 Z value 2 Density (alulated) g/m 3 F(000) 536 Number of refletions measured 5879 Number of unique refletions 1105 R int Number of observed refletions (I > 681 2σ(I)) Goodness of fit indiator Final R 1 indies [I > 2σ(I)] (R obs, wr obs ) , R indies [all data] (R all, wr all ) , Largest diff peak and hole 3.686/ e Å 3 3
4 Crystallographi data of INT-F ( 150 C) Formula I 3 Pb, C 3 H 7 NO, CH 6 N Formula weight Measurement temperature 123(2) K Crystal system monolini Spae group P2 1 / Lattie parameters a = (10) Å b = (6) Å = (3) Å α = 90 β = (7) γ = 90 Volume (6) Å 3 Z value 4 Density (alulated) g/m 3 F(000) 1200 Number of refletions measured Number of unique refletions 2528 R int Number of observed refletions (I > σ(I)) Goodness of fit indiator Final R 1 indies [I > 2σ(I)] (R obs, wr obs ) , R indies [all data] (R all, wr all ) , Largest diff peak and hole 3.305/ e Å 3 4
5 An alternative atom-to-atom mapping pathway a INT-W a b Top view C N O Pb I H solvent + solvent a b PV PVK Side view d to INT-W Pb MA + H 2 O (iodine omitted for larity) (PbI 2 ) 30 1/2 e + 30 MAI 25 C +30 H 2 O f 30 H 2 O > 30 C + 30 H 2 O 20 C a b = fiber axis INT-W motions of Pb atoms during INT-W 4.7 Å 6.3 Å I I I 2 Pb Pb I I I PVK I I 2 I Pb I Pb I I (110) normal (fiber axis) a g b PVK Figure S2. Crystal strutures of INT-W and PVK, and an alternative atom-to-atom mapping of their inter-onversion. Atomi distanes in Å in rystallographi strutures. (Top panel) (a) INT-W seen approximately along the b-axis (= fiber axis). Only two Pb sequenes are shown for larity. (b) PVK (top view). () PVK (side view). (Bottom panel) (d) Topologial illustration from PI to INT-W. (e) INT-W in Figure S1a projeted onto the ubi lattie of PVK in Figure S1b. The polymer hains extend along the b-axis perpendiular to the plane of the paper. Di-nulear strips move along the red arrows to form PVK. (f) PVK rystal lattie orrelated to INT-W in Figure S1b. Red arrows illustrate onversion to INT-W. (g) Top view of Figure S1f. The (110) normal = the b-axis of INT-W (= the fiber axis). 5
6 Referenes 1 P. Terpstra and H. G. Westenbrink, Proeedings of the Koninklijke Nederlandse Aademie van Wetenshappen 1926, 29, F. Hao, C. C. Stoumpos, Z. Liu, R. P. H. Chang and M. G. Kanatzidis, J. Am. Chem. So. 2014, 136, A. Wakamiya, M. Endo, T. Sasamori, N. Tokitoh, Y. Ogomi, S. Hayase and Y. Murata, Chem. Lett. 2014, 43, C. C. Stoumpos, C. D. Malliakas and M. G. Kanatzidis, Inorg. Chem. 2013, 52,
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