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Zeitschrift für Kristallographie - Crystalline Materials

Editor-in-Chief: Pöttgen, Rainer

Ed. by Antipov, Evgeny / Boldyreva, Elena V. / Friese, Karen / Huppertz, Hubert / Jahn, Sandro / Tiekink, E. R. T.

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Volume 210, Issue 11

Issues

Crystal and molecular structures of P,P-diphenyl-N-methyl-seleno-phosphinylthioformamide, P,P-dicyclohexyl-N-methyl-selenophosphinyl-thioformamide and P,P-dicyclohexyl-N-phenyl-selenophosphinyl-thioformamide

G. Siasios / E. R. T. Tiekink
Published Online: 2010-07-28 | DOI: https://doi.org/10.1524/zkri.1995.210.11.868

Abstract

The crystal structures of three compounds of the general formula R2P(Se)C(S)N(H)R′ have been determined at room temperature. The green crystals of [Ph2P(Se)C(S)N(H)Me], C14H14NPSSe, are triclinic, space group P[unk] with unit cell dimensions a = 12.511(3) Å, b = 13.298(3) Å, c = 10.178(3) Å, α = 109.28(2)°, β = 103.25(2)°, γ = 66.94(2)°, Z = 4 and Dx = 1.538 Mg m−3. The yellow crystals of [cHex2P(Se)C(S)N(H)Me], C14H26NPSSe, are orthorhombic, space group Pnma with unit cell dimensions a = 10.299(2) Å, b = 15.384(2) Å, c = 10.344(2) Å, Z = 4 and Dx = 1.420 Mg m−3. The yellow crystals of [cHex2P(Se)C(S)N(H)Ph], C19H28NPSSe, are triclinic, space group P[unk] with unit cell dimensions a = 9.738(2) Å, b = 11.248(2) Å, c = 9.406(1) Å, α = 100.72(1)°, β = 104.84(1)°, γ = 83.58(1)°, Z = 2 and Dx = 1.403 Mg m−3. The structures were solved by direct methods and refined by a full-matrix least-squares procedure to final R = 0.038 using 2097 reflections for [Ph2P(Se)C(S)N(H)Me], R = 0.034 using 1180 reflections for [cHex2P(Se)C(S)N(H)Me], and R = 0.033 using 2508 reflections for [cHex2P(Se) · · C(S)N(H)Ph]. The conformation about the C(1)–N(1) bond in all three structures is Z. Differences in the P(1)–C(1) and C(1)–N(1) bond distances in a series of R2P(Y)C(S)N(H)R′, Y = 0, O, S, or Se, R = Ph or cHex and R′ = Ph or Me, compounds are correlated with the nature of the phosphorus- and nitrogen-bound substituents, respectively.

About the article

Published Online: 2010-07-28

Published in Print: 1995-11-01


Citation Information: Zeitschrift für Kristallographie - Crystalline Materials, Volume 210, Issue 11, Pages 868–872, ISSN (Online) 2196-7105, ISSN (Print) 2194-4946, DOI: https://doi.org/10.1524/zkri.1995.210.11.868.

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[1]
Reinhard Kramolowsky, Jerzy Sawluk, George Siasios, and Edward R.T. Tiekink
Inorganica Chimica Acta, 1998, Volume 269, Number 2, Page 317

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