Journal ArticleDOI
Chemistry of o-xylidene–metal complexes. Part 1. o-Xylidene-magnesium reagents as metallocyclic precursors and synthesis of [Pt(CH2C6H4CH2-o)(cod)](cod = cyclo-octa-1,5-diene); the X-ray crystal structure of the macrometallocycle [{Mg(CH2C6H4CH2-o)(C4H8O)2}3]
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A high-yield synthesis of a tetrahydrofuran (thf) solution of the di-Grignard reagent (A) derived from o-bis(chloromethyl)benzene is described in this paper.Abstract:
A high-yield synthesis of a tetrahydrofuran (thf) solution of the di-Grignard reagent (A) derived from o-bis(chloromethyl)benzene is described, as well as that of an analogue obtained from 1,2-bis(chloromethyl)-4,5-dimethylbenzene. Cooling (A) to ca. –40 °C yields the colourless chloride-free Mg(CH2C6H4CH2-o)(thf) of unknown structure, whereas at ambient temperature a concentrated solution (> ca. 0.1 mol dm–3) slowly (days) deposits colourless needles of [{Mg(CH2C6H4CH2-o)(thf)2}3]. A single-crystal X-ray structure determination of the latter (R= 0.054 for 1 117 ‘observed’ reflections at 295 K) shows it to be a trimer. Crystals are orthorhombic, space group F2dd. with a= 24.706(8), b= 8.948(3), c= 44.315(9)A, and Z= 8; the trimeric unit lies on a crystallographic two-fold axis. Each of the three magnesiums is bridged to the other two by a –CH2C6H4CH2–-o ligand, the pseudo-tetrahedral co-ordination about each magnesium atom being completed by a pair of thf molecules. The utility of the di-Grignard reagent as a general metallocycle precursor is illustrated by the synthesis of [graphic omitted] (cod = cycle-octa-1,5-diene) from [Ptl2(cod)]. In contrast [PtCl2(dppe)] with [{o-C6H4(CHSiMe3)2}{Li(tmen)}2](dppe = Ph2PCH2CH2PPh2, tmen = Me2NCH2CH2NMe2) affords [Pt(dppe)2].read more
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Book ChapterDOI
X-Ray Structural Analyses of Organomagnesium Compounds
Peter R. Markies,Otto S. Akkerman,Friedrich Bickelhaupt,Wilberth J. J. Smeets,Anthony L. Spek +4 more
TL;DR: In this paper, the X-ray structural analysis of organomagnesium compounds is discussed, and it is shown that the structure of simple Grignard or diorganylmagnesium compounds tend to form polymeric structures.
Journal ArticleDOI
The chemistry of group 10 metalacycles
TL;DR: The metalacycles of Nickel, Palladium and Platinum in which the metal binds two carbon atoms form a rapidly growing class of compounds that find diverse applications in organic synthesis both in stoichiometric and catalytic reactions.
Journal ArticleDOI
Magnesium compounds: Classification and analysis of crystallographic and structural data
Clive E. Holloway,Milan Melnik +1 more
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Electronic Effects in PCP-Pincer Ru(II)-Based Hydrogen Transfer Catalysis
TL;DR: In this article, the synthesis and characterization of cyclometalated ruthenium(II) complexes [RuCl(PCPOMe)(PPh3)] and [RuCL(PCPCF3)(PPH3)] containing monoanionic, tridentate coordinating PCP-pincer ligands were reported.
Journal ArticleDOI
New preparation of benzylic aluminum and zinc organometallics by direct insertion of aluminum powder.
TL;DR: These new benzylic organometallics reacted smoothly with various electrophiles (Pd-catalyzed cross-couplings, or Cu-mediated acylation, allylations, or 1,4-addition reactions).
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