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Two samples of ∞3[Eu(Tzpy)2] were well-mixed with BN or celite (diatomaceous earth, respectively. They were then investigated by 151Eu Mössbauer spectroscopy at 78 K. The spectra of both samples show a main signal at δ, 12.9 mm s-1, which corresponds to EuII. Both samples also exhibit a weak signal at δ, 0.8 mm s-1, which corresponds to EuIII. The resulting ratio of EuII/EuIII is 80:20, which could indicate mixed valency in the compound. However, because of the air and moisture sensitivity of ∞3[Eu(Tzpy)2, the small amount of EuIII detected in the spectrum could also be caused by partial decomposition or hydrolysis. Indeed, the powder X-ray diffraction patterns of the samples used for 151Eu Mössbauer spectroscopy show weak reflections indexed to Eu2O3 and EuOOH. T
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2] are divalent (see also the Supporting Information).
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34447287622
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Crystallographic data for ∞3[Eu(Tzpy) 2, C10H6N8Eu, Mr, 390.2 g mol-1, crystal size: 0.1 x 0.1 x 0.05 mm3, space group R3c (no. 167, a1.2, 1409.9(2, c, 6940.9(6) pm, T, 170 K, Z, 36, V, 11949(3) × 106 pm3, ρcalcd, 1.952 g cm-3, 2θmax, 47.98°, STOE IPDS II diffractometer, ω scans (Δω, 2°, φ, 0.90°, MoKα radiation, λ, 0.71073 Å, 32697 reflections, 2051 unique reflections, 921 reflections with I > 2σ(I, 161 refined parameters, R1, 0.0606 (I > 2σ(I, wR 2, 0.0956 (all data, residual electron density: +1.15/-0.83 e/(106pm3, The structure was solved using direct methods SHE
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III 60.1(7). Symmetry operations: I: -y, x-y, z; II: y + 1/ 3, x-1/3, -z + 1/6; III: -x, -y, -z; IV: y, -x + y, -z; V: -x + 1/3, -x + y-1/3, -z + 1/6, VI: -x + y, -x, z.
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34447284598
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