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Study of a molybdenum dithiocarboxylato complex. Chemical characterization,crystal and molecular structure of tetrakis(α-dithionaphthoato)molybdenum(IV)
Authors:Kaluo Tang  Kassu Gebreyes  Tze -chen Hsieh  Jon Zubieta
Institution:(1) Department of Chemistry, State University of New York at Albany, 12222 Albany, New York, USA;(2) Present address: Department of Chemistry, Peking University, Beijing, The People's Republic of China
Abstract:Summary The complex Mo(agr-C10H7CS2)4 has been prepared from several starting materials: Mo(NNHPh)2(butane-2,3-diolate)2] · H2NNHPh, MoCl(NNMe2)2(PPh3)2]+Cl, MoO2 (MeCHOCHOHMe)2] · 2MeCHOHCHOHMe or (C4H9)4N]6Mo7O24, reacted withagr-C10H7CS2H. The complex Mo(agr-C10H7CS2)4 crystallizes from CH2Cl2-Et2O in the orthorhombic space group Pbca,a=13.655(3)Å,b=21.707(5)Å,c= 26.365(2)Å, V=7814.81Å3, Z=8; 5075 reflections collected, 2723 used in solution to give R=0.0517, Rw=0.0564. The molybdenum is eight coordinate with geometry approximating to aD 2d dodecahedron. The average Mo-S bond lengths are 2.526(3)Å and 2.479(3)Å for the dodecahedrala andb sites, respectively.
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