211302-19-1Relevant articles and documents
Synthesis, spectroscopic characterization, and structural studies of organogermanium tri- and monothiocarbonates. Crystal structures of Me2Ge[S2CSEt]2, Ph3Ge[SCO2Me], Ph3Ge[SCO2(i-Pr)], and Ph2Ge[SCO2Me]2
Drake, John E.,Yang, Jincai
, p. 319 - 334 (2007/10/03)
Two series of S-alkyl trithiocarbonate derivatives of dimethylgermane, Me2Ge[S2CSR]2, and halodiphenylgermane, Ph2GeX[S2CSR], where R = Me, i-Pr, n-Pr, n-Bu and X = Cl, Br, and three series of O-alkyl monothiocarbonate derivatives of triphenylgermane, Ph3Ge[SCO2R], diphenylgermane, Ph2Ge[SCO2R], and trimethylgermane, Me3Ge[SCO2R], where R = Me, i-Pr, and n-Pr, have been prepared in 73-92% yields by the reaction of the potassium or sodium salt of the appropriate tri- or monothiocarbonic acid with dichlorodimethyl-, chlorotriphenyl-, dichlorodiphenyl-, and chlorotrimethylgermane. The compounds were principally characterized by infrared, Raman, and 1H and 13C NMR spectroscopy, including some variable temperature studies, as well as by mass spectrometry. Me2Ge[S2CSEt]2, 1: P21/m (No. 11) with cell parameters a = 6.647(4) A, b = 7.423(2) A, c = 16.290(4) A, β = 91.07(3)°, V = 803.6(4) A3, Z = 2, R = 0.0484, Rw = 0.0485. Ph3Ge[SCO2Me], 13: P1 (No. 2) with cell parameters a = 9.970(4) A, b = 10.660(3) A, c = 9.853(2) A, α = 101.78(2)°, β = 109.98(2)°, γ = 89.76(3)°, V = 961.0(5) A3, Z = 2, R = 0.0534, Rw = 0.0451. Ph3Ge[SCO2(i-Pr)], 14: P1 (No. 2) with cell parameters a = 14.386(7) A, b = 18.598(6) A, c = 9.223(3) A, α = 102.85(3)°, β = 94.58(3)°, γ = 108.13(3)°, V = 2256(1) A3, Z = 2, R = 0.0545, Rw = 0.0552. Ph2Ge[SCO2Me]2, 16: Cc, (No. 9) with cell parameters a = 11.790(4) A, b = 13.696(5) A, c = 23.232(6) A, β = 92.26(3)°, V = 3748(2) A3, Z = 8, R = 0.0563, Rw = 0.0512. The immediate environment about Ge is that of tetrahedral but the orientations of the thiocarbonate groups display interesting features.