22484-01-1Relevant academic research and scientific papers
Organogermanium(IV), -tin(IV), and -lead(IV) esters of tetramethylenedithiocarbamic acid. The crystal and molecular structure of (tetramethylenedithiocarbamato)triphenyltin(IV) and -lead(IV)
Holt,Nasser,Wilson Jr.,Zuckerman
, p. 2073 - 2080 (1985)
Eight organo group 14 esters of tetramethylenedithiocarbamic acid, RnE(S2CNC4H5)4-n, where E = Ge, n = 3, and R = C2H5, E = Sn, n = 2, and R = CH3, C2H5, n-C4H9, n-C8H17, and C6H5, E = Sn, n = 3, and R = n-C4H9 and C6H5 (I), and E = Pb, n = 3, and R = C6H5 (II), have been synthesized from the ammonium salt of the carbamic acid and the group 14 chloride in methanol or chloroform and characterized by elemental analyses, physical properties, and infrared, Raman, mass, and, for the tin compounds, 119mSn M?ssbauer spectroscopies. The crystal and molecular structures of two isomorphous examples (tetramethylenedithiocarbamato)triphenyltin(IV) (I) and -lead(IV) (II) were determined. I: mp 170-173°C, C23H23NS2Sn, crystallizes in the space group Pcab with a = 23.784 (12) ?, b = 16.408 (5) ?, c = 11.346 (4) ?, V = 4427.8 (30) ?3, α = β = γ = 90.0°, Z = 8, ρcalcd = 1.488 g cm-3. II: mp 166-168°C, C23H23NPbS2, is isomorphous with a = 11.360 (3) ?, b = 23.593 (10) ?, c = 16.558 (4) ?, V = 4437.9 (25) ?3, Z = 8, ρcalcd = 1.750 g cm-3. The structures were solved from 2669 and 1720 data points, respectively, measured by ambient temperatures with monochromatic Mo Kα radiation (λ = 0.71069 ?), and refined to final R values of 5.3 (I) and 8.3% (II). The monodentate ligands give distorted Td symmetry at each metal center with bonded d(M-S) of 2.468 (3) and 2.56 (1) ? vs. nonbonded d(M?S) of 3.106 (3) and 3.26 (1) ?, respectively, for I and II.
