Synthesis and characterization of dimetallacalix[8]arene complexes
作者:Gretchen E. Hofmeister、Eugenio Alvarado、Julie A. Leary、Dong I. Yoon、Steven F. Pedersen
DOI:10.1021/ja00180a028
日期:1990.11
The one-pot synthesis of a variety of [4-tert-butylcalix [8] arene (MOR) 2 ] − [M' or R'NH 3 ] + (M=Ti, Zr, V, Sn; M'=Li, Na, K) complexes is described. The 1 H NMR spectra of these compounds possess several interesting features, including upfield shifts of α or β protons on the alkoxide ligand and a phenol hydroxyl resonance. The upfield shift is due to shielding of the alkoxide ligand by the aryl
Hydrolysis-condensation of butyltin triisopropoxide and butyltin tri-tert-amyloxide with more than three water molecules per tin atom yields only the cagelike oxo-hydroxo butyltin cluster, (BuSn)(12)O-14(OH)(6)}(OH)(2). Its molecular structure has been resolved by X-ray diffraction in the crystalline compound (BuSn)(12)(mu(3)-O)(14)(mu(2)OH)(6)}(OH)(2)(HOPri)(4). This cluster has also been characterized in solution by Sn-119, H-1, and C-13 NMR spectroscopies. The Sn-119-Sn-119/117 two bond coupling satellites oberved in the solution Sn-119 NMR spectrum have allowed measurement of four scalar coupling constants that can be correlated to the Sn-O-Sn framework. Two dimensional NMR experiments have unambiguously allowed assignment of all the H-1 and C-13 resonances of the cluster and showed that the coordination of tin is felt, at least, up to the third carbon of the butyl chains. The Sn-119 MAS NMR technique was also used to characterize solid compounds. The shielding tensorial properties are reported and discussed in relation to the oxo-hydroxo butyltin cluster structure.
Mehrotra, R. C.; Gupta, K. K., Journal of the Indian Chemical Society, 1983, vol. 60, p. 1172 - 1174
作者:Mehrotra, R. C.、Gupta, K. K.
DOI:——
日期:——
Goel, S. C.; Mehrotra, R. C., Indian Journal of Chemistry, Section A: Inorganic, Physical, Theoretical and Analytical, 1981, vol. 20, # 5, p. 440 - 442