114 - Repri nt ANGEWANDTE Volume 31[cfw]~[i!JD~...

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Volume 31 Number 9 September 1992 Pages 1253-1255 ANGEWANDTE ©[}{]~[i!JD~ International Edition in English Repri nt © VCH Verlagsgesellschaft mbH, Weinheim/Bergstr. 1992 Registered names, trademarks, etc. used in this journal, even without specific, indications thereof, are not to be considered unprotected by law. Printed in Germany Pyridine-2-thiolato Complexes of VII, VIII, and VIV with Unusual Structural Features** By John G. Reynolds,* Shawn C. Sendlinger, Ann /1'1.Murray, John C. Huffman, and George ChrislOU* One of the stimuli for our continuing interest in vanadi- um-sulfur chemistry is the relevance of this area to industrial petroleum refining. Certain crude oils contain large amounts of vanadyl (V02 +) impurities categorized into two types according to their ligands.[IJ These are the vanadyl petropor- phyrins, which have been well studied and characterized,[2J and the vanadyl nonporphyrins whose ligand environment is thought to contain S, N, and/or a donor atoms.[3J The pres- ence of these vanadyl impurities leads to the formation of [.] Prof. G. Christou, Dr. S. C. Sendlinger, Dr. J. C. HulTman Department of Chemistry and Molecular Structure Center Indiana University, Bloomington, IN 47405 (USA) Dr. J. G. Reynolds. A. M. Murray, Lawrence Livermore National Laboratory. Mail Stop L-524 P.O. Box 808 Livermore, CA 94550 (USA) [h] This work was supported by the Oflice of Basic Energy Sciences. Division of Chemical Sciences. U.S. Department of Energy. Grant DE-FG02- 87ER13702 (to G. C.) and Contract No. W-7405-ENG-48 (to J. G. R.) Al/ge'L Cirelli. II/I. Ed. EI/gi. 1992,31, So. 9 © VCH VeriagsgesellschafllllbH. W-6940 IVeinheim, 1992 0570-0833/92/0909-1253 S 3.50+.25/0 1253
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© VCH Vcrlagsgesellschafi mbH, W-6940 Weillheim. 1992 0570-0833/92/0909-125453.50 + .25/0 vanadium sulfides (primarily Y2S3 and Y3S4) under the re- ducing and sulfur-rich hydrotreating conditions.[4] These sulfides have deleterious consequences on the activity and lifetime of the heterogeneous catalyst (e.g., Mo/Co/S on alu- mina) employed for upgrading crude oil. To model the pro- gressive reduction, sulfide incorporation, and aggregation of YOz + impurities in crude oil, we have studied a variety of vanadium-sulfur compounds which contain a number of thiolato ligands and range from mono- to tetranuclear in oxidation states from III to VP -Ill More recently we have used the ligand pyridine-2-thiol (pytH) because it contains functional groups common in crude oils (thiolate Sand arene N) and also has the ability to both chelate and bridge transition metalsY ZJWe herein report the syntheses of ylI, yIIl, and ylV complexes with pyt- ligands which have unusu- al structural features; we also describe an extremely rare example of a thiolatovanadium(I1) complex. The addition of two equivalents of Na(pyt) to a solution of [VOCl2(thf)z] in THF yields the vanadium(lv) compound 1.£13JThe structure of 1 (Fig. 1)[14.23] displays an unusual bridging arragement of two pz: ~I :~Z_pyt - ligands in which the N6 atom of pyridine makes up part of the base of the square-pyramidal coordination of Yl (vertices N6, N5, S2, S3', 04) and the sulfur atom
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