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50449094885
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LiEuAsS3 (I, A mixture of Li2S (0.029 g, 0.63 mmol, Eu (0.190 g, 1.25 mmol, As (0.094 g, 1.25 mmol, and S (0.080 g, 2.50 mmol) was loaded into a fused-silica tube in a nitrogen-filled glovebox. It was flame-sealed under vacuum (∼10-4 mbar) and then heated to 650°C in 10 h. After 60 h at 650°C, it was cooled down to 250°C in 80 h followed by rapid cooling to room temperature. A mixture of red and black crystals (1:9) was obtained after dissolution of the excess flux in degassed DMF. The red crystalline phase (<10% yield) was identified as I, and the black material was mostly As. Several attempts to make pure LiEuAsS 3 have failed so far. KEuAsS3 (IIa, A red crystalline product was isolated as a single phase in >70% yield from the mixture of K2S (0.072 g, 0.66 mmol, Eu (0.100 g, 0.66 mmol, As (0.150 g, 2.00 mmol, and S (0.084 g, 2.61 mmol) using a procedure similar to that
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3.3.
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34
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50449097102
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Single-crystal X-ray diffraction data were collected at 100 K using a STOE imaging-plate diffraction system (IPDS-2) with graphite-monochromatized Mo Kα radiation. A numerical absorption correction was applied. Direct methods and full-matrix least-squares refinements against F2 were performed with the SHELXTL package. Crystal data for LiEuAsS 3 (I, monoclinic P21/c, Z, 4, a, 5.6862(5) Å, b, 13.1187(11) Å, c, 7.1735(6) Å, β, 104.858(7)°, V, 517.22(8) Å3, θmax(Mo Kα, 29.18°, total reflections, 4715, unique reflections [Fo2 > 2σFo2, 1387, number of variables, 56, μ, 19.503 mm-1, Dc, 4.238 g cm-3, Rint, 3.37, GOF, 1.427, R1, 2.45, Rw, 5.23 for
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w = 5.92 for I > 2σ (I).
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36
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50449085818
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3: Eu-S1 3.068(1), 3.069(1), 3.099(1), 3.342(1); Eu-S2 3.018(1), 3.003(1); Eu-S3 2.949(1); As-S1 2.268(1); As-S2 2.226(1); As-S3 2.223(1).
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3: Eu-S1 3.068(1), 3.069(1), 3.099(1), 3.342(1); Eu-S2 3.018(1), 3.003(1); Eu-S3 2.949(1); As-S1 2.268(1); As-S2 2.226(1); As-S3 2.223(1).
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39
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50449102152
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See the Supporting Information
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See the Supporting Information.
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