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Anne-Marie Lebuis

Publications and source records attributed to Anne-Marie Lebuis.

4 recordsLinked to original sources

Insertion of SO(2) into the S-S bond of Cp(2)MoS(2) and Cp(2)MoS(2)O to give molybdocene dithiosulfate and bis(O-alkylthiosulfates).

Cp(2)MoS(2), 3, reacts with SO(2) in CH(2)Cl(2)/EtOH mixtures to give Cp(2)MoS(3)O(2), 4, wherein the SO(2) has inserted into the S-S bond to give a dithiosulfate ligand. Crystal data for 4: P2(1)/n, a = 7.6782(6) A, b = 14.580(3) A, c = 10.2730(10) A, beta = 92.04(1) degrees, V = 1149(3) A(3), Z = 4. Cp(2)MoS(2)O, 5, reacts with SO(2) in CH(2)Cl(2) to give low yields of 4 plus other identified products. 5 reacts with SO(2) in MeOH and EtOH to give the corresponding bis(O-alkylthiosulfate), 6a and 6b, respectively. Crystal data for 6a: P 1 macro, a = 8.3226(13) A, b = 8.4736(11) A, c = 12.382(2) A, alpha = 87.803(11) degrees, beta = 77.758(11) degrees, gamma = 86.383(12) degrees, V = 851.4(2) A(3), Z = 2.

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Dicubyl disulfide.

Dicubyl disulfide (1) has been prepared in six steps from commercially available dimethyl-1,4-cubanedicarboxylate in 47% overall yield. In the final step, the previously unknown cubanethiol 2 was oxidized to disulfide 1. X-ray crystallography for 1 reveals the shortest tetragonal C-S bond on record (1.771 A). In contrast to previous generalizations, density functional theory calculations predict a low S-S rotation barrier similar to that for t-BuSSBu-t. Low-temperature (13)C NMR (600 MHz) confirms the prediction.

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Pentacarbonyl[tris[4-(methylsulfonyl)phenyl]stannyl]manganese(I): an unexpected tetragonal structure.

The title compound, [MnSn(C(7)H(7)O(2)S)(3)(CO)(5)], is asymmetric but crystallizes in the highly symmetric tetragonal space group I-4. This is achieved without the need for any disorder, either around the Sn atom or in any of the methylsulfonyl groups. The environment around the Sn atom has the following geometry: Sn-Mn = 2.6564 (7) A, mean Sn-C = 2.175 (5) A, mean C-Sn-C = 103 (2) degrees and mean C-Sn-Mn = 115 (6) degrees. The crystal packing is assisted by weak Sn.O interactions between adjacent columns of molecules, with the resulting geometry at Sn approaching highly distorted trigonal-bipyramidal.

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