154317-55-2Relevant articles and documents
Synthesis and spectroscopic characterization of S-ethyl, S-isopropyl, S-n-propyl, and S-n-butyl trithiocarbonate (trixanthate) derivatives of trimethyl- and triphenylgermane and diphenyldigermane. Crystal structure of Ph2Ge[S2CS(i-Pr)]2
Drake, John E.,Yang, Jincai
, p. 854 - 860 (2008/10/08)
The S-alkyl trithiocarbonate (trixanthate) derivatives Me3Ge[S2CSR], Ph3Ge[S2CSR], and Ph2Ge[S2CSR]2, where R = Et, i-Pr, n-Pr, and n-Bu, have been prepared in 73-85% yields by the reaction of the potassium salt of the appropriate trithiocarbonic (trixanthic) acid with iodotrimethylgermane, bromotriphenylgermane, or dichlorodiphenylgermane. The compounds were characterized by infrared, Raman, and 1H and 13C NMR spectroscopy. The crystal structure of Ph2Ge[S2CS(i-Pr)]2 was determined, and it crystallizes in space group P1 (No. 2) with the cell parameters a = 10.752(9) ?, b = 13.36(1) ?, c = 9.64(2) ?, α = 105.8(1)°, β = 113.2(1)°, γ = 91.79(9)°, V = 1211(3) ?3, and Z = 2; R = 0.0638, and Rw = 0.0626. The environment about germanium is essentially that of a distorted tetrahedron with monodentate linkages resulting in S-Ge-S and C-Ge-C angles of 87.3(2) and 118.1-(3)°, respectively, and S-Ge-C angles ranging from 110.3(3) to 113.4(3)°. The Ge-S bond distances are 2.278(5) and 2.284(5) ?, and the Ge-C bond distances are 1.925(7) and 1.941(9) ?. The terminal (C=S) sulfur atoms are oriented toward the germanium center at distances of 3.224(5) and 3.304(5) ?. All of these trixanthate derivatives are unstable as a result of the ready elimination of carbon disulfide.
