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85069021683
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K2Sm2As2Se9. A mixture of K2Se3 (0.093 g, 0.30 mmol, Sm (0.045 g, 0.30 mmol, As2Se3 (0.115 g, 0.30 mmol, and Se (0.047 g, 0.60 mmol) was loaded into a fused-silica tube in a nitrogen-filled glovebox. It was flame-sealed under vacuum (̃10-3 mbar) and then heated to 973 K within 24 h. After 5 days at 973 K, it was cooled down to 373 K at a rate of 3 K/h followed by rapid cooling to room temperature. A mixture containing black platelets (̃50% yield based on Sm) was obtained after dissolution of the excess flux in N, N′-dimethylforma-mide. Attemps to prepare pure K2Sm2As2Se9 have failed so far. K2Gd2As2Se9. Black platelets were isolated in ̃30% yield from the mixture of K2Se3 (0.078 g, 0.25 mmol, Gd (0.039 g, 0.25 mmol, As2Se3 0
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4.6.
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14
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85069023640
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Single-crystal X-ray diffraction data were collected at 170 K (Sm) and 293 K (Gd) using STOE imaging-plate diffraction systems (IPDS-1 for K 2Sm2As2Se9 and IPDS-2 for K 2Gd2As2Se9) with graphite-monochro-matized Mo Kα radiation. Numerical absorption corrections were applied. Direct methods and full-matrix least-squares refinements against F2 were carried out with the SHELXTL package. Crystal data for K2Sm2As 2Se9: orthorhombic Pnma, Z, 4, a, 17.1739(11) Å, b, 8.4628(5) Å, c, 22.6963(15) Å, V= 3298.7(4) Å3, λmax(Mo Kα, 28.05°, total reflections, 4090, unique reflections [F 02 > 2σF02, 3095, numbers of variables, 164, μ, 31.365 mm-1, D
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int= 5.80%, GOF = 1.005, Rl = 3.93% for I> 2σ(I), wR2 = 9.64 for all data.
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85172835545
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85069030788
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4 was used as a standard for 100% reflectance.
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4 was used as a standard for 100% reflectance.
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18
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0029274563
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85069021487
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