Accession Number:

ADA279701

Title:

Synthesis and Characterization of (Zn(SEt)Et)10, Formed via Insertion of Sulfur into Zn-C Bonds: A New Class of Wurtzite-like Cluster Framework

Descriptive Note:

Technical rept.

Corporate Author:

NEW MEXICO UNIV ALBUQUERQUE DEPT OF CHEMISTRY

Report Date:

1994-05-06

Pagination or Media Count:

14.0

Abstract:

The reaction of a toluene solution of ZnEt2 with one equivalent of sulfur 18 S8 results in dissolution of the sulfur to form a colorless solution. After addition of n-pentane and cooling, colorless crystals of Zn10SEt10Et10 were isolated and characterized by a variety of spectroscopic characterization techniques and by single-crystal X-ray diffraction. Crystallographic data for Zn10SEt10Et10 at 293K space group Pbar 1, a 12. 010 2A, b 14.739 3A, c 20.327 4A, a 99.93 3 deg, beta 91.62 3 deg, gamma 107.79 3 deg, V 3362.2 11 A3, Z 2, dcalc 1.636 gcu cm, R 9.41, Rw 9.00. Although the crystal deteriorated during data collection, the structural data show that Zn10SEt10Et10 exhibits a unique wurtzite-like ZnS core rather than a sphalerite-like core which is more common to zinc and cadmium alkylthiolate clusters. Thermal decomposition of Zn10SE10Et10 was studied by diffraction methods, microscopy, thermal analysis and elemental analysis. These data are consistent with the formation of a crystalline, cubic sphalerite ZnS at low temperatures, 250 deg C, providing evidence that the structure of the molecular precursor does not direct the crystallization of a particular polymorph on solid-state thermolysis in this system.

Subject Categories:

  • Inorganic Chemistry
  • Organic Chemistry
  • Physical Chemistry
  • Crystallography

Distribution Statement:

APPROVED FOR PUBLIC RELEASE