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73649125542
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Synthesis of (RAs*,RAs*, ±), RAs*,SAs*)-2: the reduction of methylenebis(phenylarsinic acid)4 with an 8-fold excess of sodium borohydride in methanol at -78 °C gave (RAs*, RAs*, ±), RAs*, S As*)-methylenebis(phenylarsine) in 53% yield after distillation. Deprotonation of the bis(secondary arsine) with 2 equiv of n-butyllithium in the presence of tetramethyl-1,2-ethylenediamine (TMEDA) gave [Li(TMEDA)]2[CH2(AsPh)2, which was isolated as a yellow crystalline solid and treated with 2 equiv of (chloromethyl) diphenylarsine6 in THF. The pure tetraarsine was isolated as a colorless liquid following elution with dichloromethane-n-hexane from a silica plate with use of a Chromatotron
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6 in THF. The pure tetraarsine was isolated as a colorless liquid following elution with dichloromethane-n-hexane from a silica plate with use of a Chromatotron.
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73649093146
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Crystal data for (RAs*,RAs*,R As*,RAs*, ±)-1: C 3H6As4O3; triclinic; space group F1̄ unit cell dimensions a, 7.3954(6) Å, b, 11.4072(10) Å, c, 11.5554(9) Å, a, 118.772(3)°, β, 90.380(3)°, γy, 90.766(3)° V= 854.30(12) Å3; Z, 4; calculated density 3.030 Mg m -3; T= 295 K; λ, 0.710 73 Å 14 095 reflections collected; 3884 independent reflections (Rint, 0.092, θmax, 27.5° absorption corrected by integration via Gaussian method implemented in maXus (2000, refinement method full-matrix least squares on F2; no. of data/parameters 3884/182; GOF, 0.99; final R1 (F2 > 2σ(F2, 0.062, wR2 F2, 0.182. All of the crystals of this compo
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2) = 0.182. All of the crystals of this compound examined were twinned. The nature of the twinning was identified and the ratio of the two components refined.
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0038864526
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Kopf, J.; von Deuten, K.; Klar, G. Inorg. Chim. Acta 1980, 55, 67.
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0001462640
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Frankenberger, W. T, Jr, Ed, Marcel Dekker: New York, Chapter 3, pp
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Francesconi, K.A.1
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