Formation, Structural Characterization, and Thermal Decomposition of the Adducts, X3Ga*P(TMS)3?X=C1,Br,I!.
DUKE UNIV DURHAM NC DEPT OF CHEMISTRY
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The adducts, X3Ga-PTMS3 X C1 1, Br 2, 13, were prepared in high yields from the combination of the respective gallium trihalides with PTMS3 in hydrocarbon solvents at ambient temperature. The adducts were characterized by NMR, MS, elemental analysis, and single-crystal X-ray stmcture determinations. Particularly, the 1H NMR study of 1-3 helped correct our previously published results regarding momomer-dimer equilibria of the related X2GaPSiMe322 in solution. The crystal structure determinations showed that 1 and 2 were solvated, 1-C6H5Cl and 2-C7H8, respectively, and that 3 was solvent-free. The thermal decomposition behavior of 1-3 was studied by TGA along with a determination of the volatiles from pyrolysis and analysis of the final solid product. The pyrolyses of 1-3 at 450 deg C under vacuum resulted in nanocrystalline GaP with 4-5 nm particle average sizes as determined by X-ray powder diffraction XRD and, for pyrolysis of 2, by transmission electron microscopy TEM in addition, small quantities of amorphous SCH containing phases were also formed.
- Inorganic Chemistry