Molecular and crystal structure of cadmium(II) diisobutyldithiocarbamate Cd[(i-C4H9)2NCS2]2 2

Autor: S. M. Zemskova, L. A. Glinskaya, R. F. Klevtsova
Rok vydání: 1999
Předmět:
Zdroj: Journal of Structural Chemistry. 40:979-983
ISSN: 1573-8779
0022-4766
DOI: 10.1007/bf02700707
Popis: i-Bu2NH ( 17 ml, 0.1 mole) was mixed with 17 ml of MeOH. and the mixture was placed in a flask cooled with an ice-NaCl mixture. CS 2 (6.0 ml, 0.1 mole) was added with vigorous stirring. Then a solution of NaOH (4.0 g, 0.I mole) in 100 ml of MeOH was dropped into the reaction mixture with cooling and stirring. The resulting clear yellowish solution was poured in portions to the solution of CdCi 2- 2.5H-,O ( 11.4 g, 0.05 mole) with stirring and cooling. A white substance precipitated in abundance from solution: it was filtered off, washed with water, and dried in air until dry to the powder state. The compound was recrystallized from a CHCI3:EtOH = 1:1 (v/v) mixture, Yield 24.4 g (94%), mp 172~ The metal content was measured (by trilonometric titration) to be 21.6% (calculated 21.6%). The single crystals of [Cd(i-Bu2NCS2)2] 2 were ~own by slowly cooling the hot saturated solution in toluene and subsequently evaporating it at room temperature. Transparent light yellow crystals were selected for X-ray diffraction analysis. One of the single crystals, sized ().Ix 0.2x 0.2 ram, was used for data collection (5226 reflections). The intensities were measured on a CAD-4 Enraf-Nonius automatic diffractometer using the standard procedure (~r m 0/20 scan mode, variable scan speed, ~aphite monochromator, maximal 20= 50~ The data were corrected for empirical (azimuthal q~ scan) absorption, /a(MoKc0 = 11.87 cm-1. The crystals are monoclinic with unit cell parameters a= 50.087(11), b= 9.613(2), c= 23,708(8) ,A, [3= 116.51(2)~ V= 10,215 A3 Z = 18; dcatc= 1.355 ~cm 3. The space group C2/c was determined by analyzing the extinctions in Fhk I and confirmed by further calculations. The structure was solved by direct methods with the SHELXS-86 pro~am [2] and refined by the full-matrix least-squares procedure anisotropically tor nonhydrogens with the SHELXL-93 program complex [3]. All hydrogen atoms were placed geometrically and included in the refinement in the isotropic approximation. The final R value (H atoms included) is 0.0466 for 5156 independent F,~t! with I > 20(1) (495 refined parameters). The corresponding positional and equivalent thermal isotropic parameters of basic atoms are given in Table 1; selected bond lengths and angles, in Table 2. The
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