4926
lnorg. Chem. 1995, 34, 4926-4929
A New Three Dimensional Crystal Structure of a Cadmium Thiolate
Table 1. Crystallographic Data for 1 formula fw space group
Tobias Vossmeyer, Gunter Reck,’ Lynne Katsikas,’ Erhard T. K. Haupt,$ Burkhard Schulz? and Horst Weller*J’
a,
c. A
v. A‘
Z
Hahn-Meitner-Institut, Abteilung Kleinteilchenforschung, Glienicker Strasse 100, 14109 Berlin, Germany
ecBic,g cm-’ u(Mo Ka), cm-I yj-scan abs corr transm factors T, “C i, A Ri(F,,)“” RdF,’)’
Received January 27, 1995
Introduction X-ray structure investigations on the class of nonmolecular compounds Cd(SC6H4X)Z have revealed that the nature and position of the substituent X have a decisive influence on the crystal structure. Thus, with X = H, CH3-4, or CH3-2, different three dimensional structures are obtained’-’ whereas with X = Br-4 a two dimensional crystal structure is r e a l i ~ e d .However, ~ to the best of our knowledge, only one and two dimensional structures of cadmium thiolates with aliphatic residues have until now been described. Examples are the crystal structures of Cd(SCH2COOCH2CH&5and Cd(SCH2CHZ0H)26built up of linear chains or layers, respectively. In this article we present a three dimensional nonmolecular structure of a cadmium thiolate with an aliphatic ligand (C~(SCH~CH(OH)CHZOH)~, 1) which was crystallized from an aqueous solution of cadmium perchlorate and 1-thioglycerol.
Experimental Section General Details. All chemicals used were of analytical grade or of the highest purity available and obtained from Alfa, Fluka, and Merck. X-ray powder diffraction was carried out using a Siemens D 5000 diffractometer operating with a Cy anode. A nickel filter was used to select the K a lines (1 = 1.506 A). I’jCd-NMR spectra were recorded with a Varian Gemini-200 BB spectrometer (4.7 T) at 44.4 MHz. As ref ilcdci? = 98 ppm (1.0 M aqueous solution) was taken which corresponds to acdrcio,,? = 0 ppm (0.1 M aqueous solution).7 Elemental analysis was carried out commercially at the microanalytic laboratory Pascher in Remagen-Bahndorf, Germany. Preparation of Cd(SCH2CH(OH)CH20H)2. Two different methods were used: A) 2.0 g (4.8 mmol) of Cd(C10&.6H?O and 1 mL ( I 1.5 mmol j of I-thioglycerol were dissolved in 250 mL of deionized water. The solution was adjusted to pH 11.2 using 1 M NaOH and dialyzed two times against I O L of deionized water (using spectrapor MWCO 3500 dialysis tubings). As the pH value of the solution slowly decreased. colorless crystals grow in the dialysis tubings as flat tetragonal bipyramids. These crystals were used for X-ray structure ~~
~
*To whom correspondence should be addressed. ‘Permanent address: Bundesanstalt fur Materialforschung und -ptfifung, Berlin. Germany. -Permanenr address: Faculty of Technology and Metallurgy. University of Belgrade. Belgrade. Yugoslavia. “Permanent address: Institut fur Anorganische und Angewandte Chemie. Universitat Hamburg. Hamburg. Germany. l 1 Permanent address: Institut fur Physikalische Chemie. Universitat Hamburg. Bundesstrasse 45. 20146 Hamburg, Germany. ( I ) Craig. D.: Dance. I. G.: Garbutt. R. .4n,qew Chenz. 1986. 98. 178: A n p ~ t Chem.. . Inr. Ed. En
