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1 Supporting Information Wiley-VCH Weinheim, Germany
2 Supplementary Online Data Reversible Redox Reactions in an Extended Polyoxometalate Framework Solid Chris Ritchie 1, Carsten Streb 1, Johannes Thiel 1, Scott G. Mitchell 1, Haralampos N. Miras 1, De-Liang Long 1, Thomas Boyd 1, Robert D. Peacock 1, Thomas McGlone 1, and Leroy Cronin 1 * L.Cronin@chem.gla.ac.uk ; website: 1 WestCHEM, Department of Chemistry, The University of Glasgow, Glasgow, G12 8QQ, UK *To whom correspondence should be addressed General Materials and Methods K 8 [γ-siw 10 O 36 ].12H 2 O was synthesized using a published procedure: A. Tézé, G. Hervé, Inorganic Syntheses, A. P. Ginsberg, Ed. (John Wiley & Sons, New York, 1990), Vol. 27, pp The purity of the starting materials was confirmed by FT-IR. All other materials were purchased from Sigma Aldrich Chemicals and used without further purification. Fourier-transform infrared (FT-IR) spectroscopy: Unless stated otherwise, the materials were prepared as KBr pellets and FT-IR spectra were collected in transmission mode using a JASCO FT-IR- 410 spectrometer or a JASCO FT-IR 4100 spectrometer. Wavenumbers (ν) are given in cm -1 ; intensities as denoted as wk = weak, m = medium, s = strong, br = broad, sh = sharp. Microanalysis: Carbon, nitrogen and hydrogen content were determined by the microanalysis services within the Department of Chemistry, University of Glasgow using an EA 1110 CHNS, CE-440 Elemental Analyzer. Flame Atomic Absorption Spectrometry (FAAS): FAAS was performed at the Environmental Chemistry Section, Department of Chemistry, University of Glasgow on a Perkin-Elmer 1100B Atomic Absorption Spectrophotometer. Single crystal X-Ray diffraction: Single crystal datasets were collected at 150(2) K unless stated otherwise on the following instruments: Rigaku Spider Image Plate System (λ (Mo Kα ) = Å) (Compound 1 ox ); Oxford Diffraction Gemini Ultra S (λ (Mo Kα ) = Å) (Compound 1 red ). Powder X-Ray diffraction (XRD): Powder XRD patterns were collected on a Bruker AXS D8 powder diffractometer (λ(cu Kα ) = Å) equipped with a graphite monochromator. Unless stated otherwise the datasets were collected in capillary mode at room temperature. UV-Vis spectroscopy: UV-Vis spectra were collected using a Shimadzu PharmaSpec UV-1700 UV-Vis spectrophotometer in transmission mode using quartz cuvettes with 1.0 cm optical path length. 1 H-Nuclear magnetic resonance spectroscopy ( 1 H-NMR): 1 H-NMR spectroscopy was performed on a Bruker DPX 400 spectrometer using the solvent signal as internal standard. All δ values are given in ppm. 1
3 Thermogravimetric analysis (TGA): Thermogravimetric analysis was performed on a TA Instruments Q 500 Thermogravimetric Analyzer under nitrogen flow at a typical heating rate of 5 C min -1. Differential scanning calorimetric analysis (DSC): DSC analysis was performed on a TA Instruments Q 200 calorimeter under nitrogen flow at a typical heating rate of 10 C min -1. Syntheses and Analysis Compound 1 ox : POM-1MnSi - (C 4 H 10 NO) 40 [W 72 Mn III 12O 268 Si 7 ].48H 2 O Morpholine (9.0 g, 103 mmol) was added to 200 ml of a 1M aqueous NaCl solution and the ph was subsequently adjusted to 8.0 using 4.5 M H 2 SO 4. At this point fresh air dried K 8 SiW 10 O H 2 O (1.486 g, 0.50 mmol) was added under vigorous stirring until fully dissolved. Solid MnSO 4. H 2 O (127 mg, 0.75 mmol) is then added resulting in a bright yellow solution and the ph is adjusted to 7.80 using 4.5 M H 2 SO 4. KMnO 4 (24 mg, 0.15 mmol) is then added slowly and the solution is stirred for a further 5 min. At this point a deep brown solution is obtained which is then centrifuged to remove any insoluble material. Finally the ph of the solution is adjusted to 7.75 using 4.5 M H 2 SO 4. Tetrahedral diffraction quality crystals begin to form after 2 weeks. Yield after 1 month = 350 mg (15.4 µmol, 22.12% based on W). Elemental analysis for (C 4 H 10 NO) 40 [W 72 Mn 12 O 268 Si 7 ]. 48H 2 O, C 160 H 496 N 40 Mn 12 O 356 Si 7 W 72, Mw = g/mol -1 calcd (found) : C 8.44, (8.79); H 2.20, (2.16); N 2.46, (2.50); W 58.13, (58.01); Mn 2.90, (2.95). FT-IR (KBr) ν/cm (m), 1453(sh), 1310(sh), 1102(sh), 1042(sh), 984(sh), 900(sh), 737(br). UV-Vis λ max = 480 nm, ε = 2.38x10 4 L -1 mol -1 cm Crystal data and structure refinement for 1 ox : [C 160 H 496 N 40 Mn 12 O 356 Si 7 W 72 ], M r = g mol 1 ; a tetrahedral brown crystal ( mm 3 ) was analyzed with a Rigaku Image Plate diffractometer using Mo-K α radiation (λ = Å) at 150(2) K. Cubic, space group I-43d, a = (5) Å, V = 57249(12) Å 3, Z = 4, ρ = g cm 3, µ(mo Kα ) = mm 1, F(000) = 41240, reflections measured, of which 6229 are independent, 364 refined parameters, R1 = , wr2 = Many data sets were collected of the native material, and the material returned to the oxidized state during the redox cycles and the average unit cell parameter was 38.54(4) with a maximum variation of ± 0.02 Å. CCDC reference
4 Compound 1 ox : Thermal analysis Fig. S1. Thermal gravimetric analysis of 1 ox showing the loss of solvent water (RT- 100 C) followed by the decomposition of the morpholine counterions ( C) and framework collapse at 563 C. Fig. S2. Differential scanning calorimetry plot of 1 ox, showing framework collapse at 563 C in correlation with TGA analysis. 3
5 Compound 1 red : (C 4 H 10 NO) 40 H 12 [W 72 Mn II 12O 268 Si 7 ].48H 2 O 20 mg (0.88 µmol) of air dried 1 ox is added to 5 ml MeOH in which it is completely insoluble. 10 mg (56.8 µmol) of L-ascorbic acid is then added which dissolves over the course of a few minutes. Within 60 minutes the reduction of Mn(III) to Mn(II) in 1 ox is complete with retention of the crystallinity of the material resulting in the SC-SC transformation and generation of 1 red. This transformation is confirmed by collection of a second single crystal data set which shows elongation of the [W-O-Mn] distances in accordance with reduction of Mn III to Mn II (CCDC reference no ). Furthermore the reduction results in a significant expansion of the unit cell volume by more than 3100 Å 3, corresponding to ca. 5.5 vol.-%. The redox reaction can be followed visually by a change in crystal colour from deep red-brown (Mn(III)) to pale yellow (Mn(II)). UV-Vis spectroscopy confirms this reduction reaction. The absorption maximum for Mn(III) at λ max = 480 nm disappears and two new signals at λ max, 1 = 350 nm and λ max, 2 = 373 nm appear which are characteristic for Mn(II). Potentiometric redox titrations of the solid material using Ce IV (SO 4 ) 2 in sulphuric acid demonstrate that all Mn centers present are Mn(II). Elemental analysis for (C 4 H 10 NO) 40 H 12 [W 72 Mn 12 O 268 Si 7 ].48H 2 O, C 160 H 508 Mn 12 N 40 O 356 Si 7 W 72, Mw = g/mol -1 calcd (found): C 8.44, (8.94); H 2.20, (2.38); N 2.46, (2.42); W 58.13, (55.00); Mn 2.90, (2.81).The increase in carbon content is most likely associated with the uptake of L-ascorbic acid into the structural voids. FT- IR (KBr) ν/cm (s), 2849(s), 1599(wk), 1457(s), 1374(m), 1302(w), 1106(w), 1041 (wk), 947 (wk), 890 (wk), 717 (m). Crystal data and structure refinement for 1 red : [C 160 H 508 Mn 12 N 40 O 356 Si 7 W 72 ], M r = g mol 1 ; a yellow tetrahedral crystal ( mm 3 ) was analyzed with an Oxford Diffraction Gemini Ultra diffractometer using Mo-K α radiation (λ = Å) at 150(2) K. Cubic, space group I-43d, a = (5) Å, V = (13) Å 3, Z = 4, ρ = g cm 3, µ(mo Kα ) = mm 1, F(000) = 41288, reflections measured, of which 4692 are independent, 352 refined parameters, R1 = , wr2 = Many data sets were collected during the redox cycles and the average unit cell parameter was 39.21(4) with a maximum variation of CCDC reference Percentage Difference Compound 1 ox Compound 1 red Difference (1 red -1 ox ) (1 red -1 ox ) / % a/å (5) (1) V/Å (12) (13) Table S1: Comparison of the unit cell parameters of compound 1 ox and 1 red 4
6 Fig. S3. Left: 1 H-NMR experiment showing the gradual oxidation of ascorbic acid (A) to dehydroascorbic acid 2-methyl hemi-ketal (B). Right: A schematic illustrating the single-crystal to singlecrystal redox transformation from 1 ox to 1 red. The framework of POM-1 (top center; 3-connected nodes: green, 4-connected nodes: red, internal void: yellow ellipsoid) can be reversibly switched from a fully oxidized state (1 ox, left) to a fully reduced state (1 red, right) under framework expansion from a unit cell volume of 57,249 Å 3 to Å 3. The photographic inserts illustrate the change in crystal colour from the oxidized form (1 ox, red-brown) to the reduced form (1 red, light yellow). The switching process is complete for both 1 ox to 1 red and 1 red to 1 ox within 30 min. when the concentration of the ascorbic acid and mcpba is 10 mm for each process respectively. Recrystallization of Compound 1 ox and re-oxidation of 1 red in aqueous solution Compound 1 ox is soluble in hot water (ca. 20 mg / ml). If compound 1 ox is dissolved in an aqueous solution, and allowed to cool over a 20 hour period, compound 1 ox re-crystallizes as the native material, forming brown tetrahedral crystals of identical size and shape, see Fig. S4. Similar experiments with compound 1 red showed that 1red can also be dissolved in hot water. However, recrystallization of 1 red over a period of several weeks resulted in the formation of brown tetrahedral crystals of compound 1 ox. The process can be described as the dis-assembly of 1 red with consecutive air oxidation of the Mn II centres in solution to Mn III and re-crystallization of the fully oxidized compound 1 ox. Single crystal unit cell determinations on the crystals confirm these observations. Fig. S4. Micrograph of an aqueous solution of compound 1 ox in a well plate (left) and the re-crystallized product obtained after 20 h (right). The tetrahedral crystal habit can clearly be seen. A supplementary video of this process is also available on request. 5
7 Compound 1 red : Thermal analysis Fig. S5: Thermal gravimetric analysis of 1 red, showing the loss of solvent water (RT- 100 C) followed by the decomposition of the morpholine counterions ( C). Fig. S6: Differential scanning calorimetry plot of 1 red, showing framework collapse between C. 6
8 Fig. S7: Powder X-ray diffraction pattern of compound 1 ox (red line) and the simulated powder X-ray diffraction pattern calculated from single crystal diffraction data (blue line). Comparison shows the purity of the bulk sample. 7
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