Original scientific paper

Synthesis and Characterization of trans-(pyH)[Mo(NCS)₄py₂] and trans-(py₂H)[Mo(NCS)₄py₂]. Crystal Structure of trans-(py₂H)[Mo(NCS)₄py₂]

Nives Kitanovski ; University of Ljubljana, Faculty of Chemistry and Chemical Technology, Aškerčeva 5, 1001 Ljubljana, Slovenia
Amalija Golobić ; University of Ljubljana, Faculty of Chemistry and Chemical Technology, Aškerčeva 5, 1001 Ljubljana, Slovenia
Boris Čeh ; University of Ljubljana, Faculty of Chemistry and Chemical Technology, Aškerčeva 5, 1001 Ljubljana, Slovenia

Abstract

(pyH)[Mo(NCS)₄py₂] (1) (py = pyridine) was prepared by refluxing of the mixture of KSCN and [MoCl₃py₃] in pyridine. After the recrystallization of 1 in pyridine, single crystals of trans-(py₂H)[Mo(NCS)₄py₂] (2) were obtained. X-ray structure determination of 2 reveals trans slightly elongated (4 + 2) octahedral arrangement of two staggered conformated (85.9(4)°) N-bond pyridine molecules (Mo–N(py) = 2.191(6), 2.176(5) Å) and four isothiocyanato groups in square-planar orientation, bonded within the range 2.083(7)–2.106(7) Å to molybdenum atom in the anion. In the (py₂H)+ cation, pyridine molecules are held together by a strong hydrogen bond with contact distance N7…N8 = 2.708(12) Å (N8–H8'…N7 geometry: N8–H8'…N7 = 175(7)°, N7…H8' = 1.65(7) Å, N8–H8' = 1.06(7) Å). The angle between the best planes through the pyridine–cation rings is 70.7(6)°. The results of IR and UV/Vis spectroscopy indicate the same arrangement of the ligands in the compounds 1 and 2.

Keywords

molybdenum(III); isothiocyanates; pyridine; crystal structure

Hrčak ID:

102983

URI

https://hrcak.srce.hr/102983

Publication date:

30.11.2004.

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